CN103102705B - Asphalt composition particle and preparation method thereof - Google Patents
Asphalt composition particle and preparation method thereof Download PDFInfo
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- CN103102705B CN103102705B CN201110353558.4A CN201110353558A CN103102705B CN 103102705 B CN103102705 B CN 103102705B CN 201110353558 A CN201110353558 A CN 201110353558A CN 103102705 B CN103102705 B CN 103102705B
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Abstract
The invention provides an asphalt composition particle and a preparation method thereof. The preparation method comprises the following steps: selecting a base asphalt raw material with a proper softening point and adding the base asphalt raw material and a proper solid dispersant into a crushing apparatus for pre-dispersion; placing the pre-dispersed material in a low temperature environment until the material is embrittled, taking out the embrittled material and carrying out crushing immediately; adjusting the particle size of asphalt through controlling different refrigeration time and temperature and crushing time; and finally a small amount of a coating agent is added and carrying out mixing for a short time so as to prepare the asphalt composition particle with excellent high temperature performance and resistance to temperature sensitivity, a fine particle size, suitability for normal temperature storage and a high softening point. The asphalt composition particle with a high softening point prepared by using the preparation method in the invention has a particle size of less than 120 mm and is free of caking.
Description
Technical field
The present invention relates to a kind of Asphalt composition particle and preparation method, relate in particular to a kind of high softening point bitumen composition of oil field welldrilling and the method for preparation.
Background technology
High softening point bitumen refers to that softening temperature is more than 100 DEG C, the pitch especially more than 120 DEG C.High softening point bitumen has because of its outstanding high-temperature resistance to be applied more widely.As the use of the roof cover as building, even trickle even if also can not become very soft during the broiling summer.Can also be used in the drilling operation in deep-seated oil gas field, as the important component part of drilling fluid, shutoff, anti-collapse, stabilizing borehole, the effect of reduced rate filter loss can be played under the high temperature conditions.In addition, the property-modifying additive etc. of macromolecular material can also be used as.
Asphalt product has purposes widely in oil/gas drilling process, can as the important component part of drilling fluid (being commonly called as mud), be one of indispensable important dose of kind of domestic and international modern drilling engineering, there is good anti-collapse, lubrication, comprehensive effectiveness such as reduction leak-off and high-temperature stable etc.Along with the development of Petroleum finance, drilling depth is constantly deepened, and drilling strata is more and more complicated, and the quantity of the special well such as orientation well, horizontal well increases gradually.This makes drilling engineering have higher requirement to drilling fluid asphalt product and system thereof.Common softening point asphalt can cannot meet the high-temperature service requirement under deep-well because overbating even trickling.Develop the high softening point bitumen that high-temperature behavior is good, have good seal-off effect and filtration reduction, to meet the needs of oil drilling engineering, tool is of great significance.
In order to improve the use properties of drilling fluid asphalt product, successively disclosing a lot of method carries out modification to pitch both at home and abroad.Wherein topmost method just carries out sulfonation to pitch.As US3485745, CN99109453, CN201010250241 etc.Although this method can increase the water-soluble of product, oil solution ratio is lower.Pitch mainly generates sulfonate after sulfonation, and the softening temperature of product does not almost measure, and can only use under lower temperature condition.And its particle does not have elasticity, deformability poor, the duct in well can not be embedded arbitrarily, particularly irregular shape duct, the effect of shutoff and filtrate reducing can not be played well.Meanwhile, this technique is more complicated, easily pollutes environment.CN99123211 discloses a kind of method adopting the method production well plugging agent of surface portion sulfonation, and the advantage of this method is the molten thing content of oil (can reach 60%) that improve product, thus improves the content of deformable particle in product.Shortcoming is that the softening temperature of product only has about 100 DEG C, cannot use in deep-well and ultra deep well.
When high softening point bitumen uses in drilling fluid, require with small Granular composite in mud system, so both can ensure that pitch is uniformly dispersed, can avoid again being agglomerated into larger block blocking vibration sieve and cause the generation of problems such as cannot using.Under normal circumstances, the Particle size requirements of pitch particle is below 120 μm, and even less than 100 μm can normally use.
But it is very difficult for asphalt powder being broken into little particle.Adopt general disintegrating apparatus the material of building stones or coal class can be ground into very little particle.But pitch and above-mentioned substance have very large difference.Because in crushing process, produce a large amount of heat along with the high speed rotating of pulverizer and material friction, temperature of charge can be made to raise a lot.Pitch due to its special physical property, can along with temperature rising deliquescing, become sticky, even if pulverized small-particle also can be bonded to large particle again.And the particle diameter pulverized is less, this situation is more obvious.
In order to address these problems, CN95120535 discloses a kind of method of producing high softening point bitumen fine particle.It mainly comprises three steps: first raw material and water are made emulsion, then extracts from the fine particle of emulsion and removes light constituent, is finally separated and reclaims pitch fine particle.The method can obtain tiny pitch particle, and shortcoming is complex technical process, needs to use a large amount of organic solvent during extraction, and production cost improves.In the end recovery treatment stage needs drying, easily causes pitch particle partial melting and is again bonded together.
CN200310107024 discloses a kind of production method of granular pitch, comprises thermal spraying and freezing crushing method two kinds.Thermal spraying is by after massive asphalt heating and melting, and by high-pressure nozzle from cooling tower top Jet with downward flow direction, cooling tower bottom side constantly upwards sprays subcooling gas, and make the pitch nebulized form particle through cooling, drying obtains.This method is inapplicable to high softening point bitumen.Because high softening point bitumen is instant, viscosity is also very high at relatively high temperatures, easily causes spray nozzle clogging, the problem such as cannot to spray.
Freezing and pulverizing technology is risen at the beginning of last century, is first applied at rubber and plastic industry.Freezing and pulverizing utilizes material " fragility " at low temperatures, and namely material is along with the reduction of temperature, and its hardness and fragility increase, and plasticity and toughness reduce.Freezing and pulverizing principle is exactly first material is chilled to below glass transition temp or embrittlement temperature, then uses less power namely can by crushing material.This method is a kind of more satisfactory grinding mode for coal-tar pitch, but for petroleum pitch, particularly high softening point bitumen exists larger problem.Petroleum pitch has special sticky toughness and temperature sensitivity, only adopts freezing and pulverizing that pitch particle degree can be caused inadequate.Even if pitch granularity can reach requirement, but diminishing along with pitch particle diameter, and specific surface area increases, and presents autohemagglutination trend, also cannot preserve for a long time at normal temperatures between particle.
Summary of the invention
The grain diameter existed in production high softening point bitumen particle process for prior art is large, easily again block is bonded to after pulverizing, the problem such as can not to store for a long time at normal temperatures, the invention provides a kind of by selecting suitable basic asphalt, add different additives, adopt the method for pre-dispersed-freezing-pulverizing to produce high softening point bitumen composition grain.Present invention process is simple, easy to operate, cost is lower, and products obtained therefrom not only grain diameter is little, and high-temperature behavior and anti-temperature-sensitive excellent property, can meet high-temperature drilling job requirements.
Asphalt composition particle of the present invention, by mass percentage, comprises following component:
(1) basic asphalt: 70% ~ 94.5%;
(2) solid dispersion: 5% ~ 29.5%;
(3) coating agent: 0.1% ~ 5%;
The mean particle size of Asphalt composition particle is 10 ~ 120mm, is preferably 30 ~ 100mm.
In bituminous composition of the present invention, the softening temperature of basic asphalt is more than 120 DEG C, preferably more than 150 DEG C, is generally 120 ~ 220 DEG C, is preferably 150 ~ 190 DEG C.Basic asphalt can be oxidized bitumen and/or solvent deoiling pitch, and be preferably the mixture of oxidized bitumen and solvent deoiling pitch, wherein oxidized bitumen accounts for 30% ~ 70% of basic asphalt quality, and solvent deoiling pitch accounts for 70% ~ 30% of basic asphalt quality.The mass percentage of basic asphalt in bituminous composition is preferably 75% ~ 89%.
In bituminous composition of the present invention, solid dispersion is one or more in graphite, polynite and wilkinite.Add-on preferably accounts for 10% ~ 20% of bituminous composition total mass.Solid dispersion is pulverulence.
In bituminous composition of the present invention, coating agent be water soluble resin, polyvinylpyrrolidone (PVP) one or more.Water soluble resin is as water soluble acrylic resin, water soluble alkyd resin, Polyester Resin Water Soluble etc.Solid dispersion and coating agent can use commercial goods.
In bituminous composition of the present invention, suitable auxiliary agent can also be added as required, as antioxidant, softening agent etc., specifically can be determined by those of ordinary skill in the art according to the requirement of use properties.
The preparation method of Asphalt composition particle of the present invention comprises following process: select basic asphalt raw material (being generally block), basic asphalt raw material and solid dispersion are joined in disintegrating apparatus and carries out pre-mixing dispersion, then low temperature environment is placed in brittle to material, temperature is 0 ~-60 DEG C, be preferably-10 ~-30 DEG C, time is 2 ~ 48 hours, is preferably 2 ~ 10 hours; After low temperature brittleness, material is pulverized in disintegrating apparatus, then adds coating agent, mixes, and namely prepares high softening point bitumen composition grain.
In the above-mentioned preparation method of the present invention, disintegrating apparatus can be high energy shear milling machine, colloidal mill or jaw crusher.Add the mixing process after coating agent also to carry out in disintegrating apparatus.Also can adopt suitable equipment, in crushing process, carry out cooling operation.
In the above-mentioned preparation method of the present invention, during pre-mixing dispersion, charging is normal temperature, and pre-mixing jitter time is 1 ~ 10s, and after low temperature brittleness, the grinding time of material is 10 ~ 40 s, and adding the mixing time after coating agent is 1 ~ 10s.
The inventive method can prepare high-temperature behavior and anti-temperature-sensitive excellent property, and particle diameter is adjustable, is applicable to the high softening point bitumen composition grain of normal temperature long storage periods (not boning).Asphalt composition particle of the present invention is suitable for prepares drilling fluid.
In the inventive method, first select oxidized bitumen and the solvent deoiling pitch of suitable softening temperature, in the mixing of suitable ratio.Based on selecting the pitch of two kinds of different process, pitch has obvious advantage, and the oxidized bitumen that softening temperature is close and solution-off pitch, character is not identical.Oxidized bitumen toughness is comparatively large, not easily pulverizes and disperses, but viscosity with temperature change is not fairly obvious, has good resisting temperature susceptibility; Solution-off ductility of bitumen is less, and comparatively easily pulverize and dispersion, but viscosity with temperature changes greatly, resisting temperature susceptibility is relatively poor.Both employings are composite, can learn from other's strong points to offset one's weaknesses, and reach better use properties.
In the inventive method, solid dispersion mainly comprises one or more in graphite, polynite and wilkinite.Wherein graphite not only can contribute to dispersion and the pulverizing of high softening point bitumen, and can play lubrication when this bituminous composition is applied in the middle of drilling fluid, is conducive to the generation preventing the accidents such as bit freezing.And the integral part of polynite, wilkinite inherently drilling fluid, so do not introduce other inorganic inert component, the destruction of drilling mud system also just can not be caused.
In freezing and pulverizing process, freezing object allows the fragility of material increase, and plasticity and sticky toughness reduce, and so namely use less power just can reach good crushing effect.But crushing process can release a large amount of heat due to frictional impact, very easily causes the bonding again of pitch particle, the present invention adopt freezing-method pulverized in short-term can avoid the generation of this kind of problem.In addition, the pitch particle for drilling fluid is not better less.Because pitch particle in use, certain deformation occurs along with the rising of temperature, different formation fractures and duct, the grain diameter of requirement is different.This step is the Main Means that grain size regulates.The size of pitch particle can be adjusted by controlling freezing time, freezing temp and grinding time, thus meet different service requirementss.
For petroleum pitch particularly high softening-point petroleum pitch, still have problems only by the technique adding dispersion agent freezing and pulverizing.Crushing material can be obtained very thin at low temperatures, but along with material specific surface area increase, present autohemagglutination trend between particle, the preceding paragraph time will be combined into block excessively at normal temperatures, cannot preserve for a long time at normal temperatures.And particle diameter is less, this situation is more obvious.The present invention adds a small amount of coating agent in fine particle, then mixes instantaneously.Coating agent also claims separant, and trickle pitch particle can wrap by it, and pitch particle is kept apart.Can not coalesce together at normal temperatures, therefore solve storage at normal temperature problem.
Embodiment
To be further described the present invention by embodiment below, but not thereby limiting the invention, and percentage composition is wherein mass percentage.
Embodiment 1
By the oxidized bitumen that softening temperature is 152.0 DEG C, account for 35% of basic asphalt, and softening temperature is the solution-off pitch of 153.2 DEG C, account for 65% of basic asphalt, join in high speed disintegrator with the graphite accounting for total material 18%, mixing time 4s, put into refrigerator-freezer freezing temp-20 DEG C, freezing 8 hours, then pulverize, grinding time 20s, add the water soluble acrylic resin accounting for material total amount 1.2%, remix 6s, obtains high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Comparative example 1
By the oxidized bitumen that softening temperature is 152.0 DEG C, account for 35% of basic asphalt, with the solution-off pitch that softening temperature is 153.2 DEG C, account for 65% of basic asphalt, join in high speed disintegrator with the graphite accounting for total material 18%, mixing time 4s, put into refrigerator-freezer freezing temp-20 DEG C, freezing 8 hours, grinding time 20s, obtained high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Embodiment 2
By the oxidized bitumen that softening temperature is 164.5 DEG C, account for 30% of basic asphalt, and softening temperature is the solution-off pitch of 161.8 DEG C, account for 70% of basic asphalt, with account for the graphite of total material 18% and account for the wilkinite of total material 6%, join in high speed disintegrator, mixing time 5s, put into refrigerator-freezer freezing temp-25 DEG C, freezing 10 hours, grinding time 25s, added the water soluble alkyd resin accounting for material total amount 1.0%, remix 5s, obtains high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Comparative example 2
By the oxidized bitumen that softening temperature is 164.5 DEG C, account for 30% of basic asphalt, with the solution-off pitch that softening temperature is 161.8 DEG C, account for 70% of basic asphalt, put into refrigerator-freezer freezing temp-25 DEG C, freezing 10 hours, grinding time 25s, add the water soluble alkyd resin accounting for material total amount 1.0%, remix 5s, obtain high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Embodiment 3
By the oxidized bitumen that softening temperature is 176.2 DEG C, account for 55% of basic asphalt, and softening temperature is the solution-off pitch of 174.8 DEG C, account for 45% of basic asphalt, with account for the graphite of total material 10% and account for the wilkinite of total material 4%, the polynite of total material 4% joins in high speed disintegrator, mixing time 5s, put into refrigerator-freezer freezing temp-30 DEG C, freezing 10 hours, grinding time 35s, added the polyvinylpyrrolidone accounting for material total amount 1.5%, remix 7s, obtains high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Comparative example 3
By the oxidized bitumen that softening temperature is 176.2 DEG C, account for 55% of basic asphalt, and softening temperature is the solution-off pitch of 174.8 DEG C, account for 45% of basic asphalt, with account for the graphite of total material 10% and account for the wilkinite of total material 4%, the polynite of total material 4% joins in high speed disintegrator, mixing time 5s, put into refrigerator-freezer freezing temp-10 DEG C, freezing 4 hours, grinding time 35s, added the polyvinylpyrrolidone accounting for material total amount 1.5%, remix 7s, obtains high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Embodiment 4
By the oxidized bitumen that softening temperature is 185.2 DEG C, account for 65% of basic asphalt, and softening temperature is the solution-off pitch of 186.6 DEG C, accounts for 35% of basic asphalt, join in high speed disintegrator with the graphite accounting for total material 20%, mixing time 5s, puts into refrigerator-freezer freezing temp-25 DEG C, freezing 6 hours, grinding time 35s, add the polyvinylpyrrolidone accounting for material total amount 1.8%, remix 8s, obtain high softening point bitumen composition grain.Normal temperature stacks 30 days, sieves.
Comparative example 4
By the oxidized bitumen that softening temperature is 185.2 DEG C, account for 65% of basic asphalt, with the solution-off pitch that softening temperature is 186.6 DEG C, account for 35% of basic asphalt, join in high speed disintegrator with the graphite accounting for total material 20%, directly pulverize, grinding time 25s, add the polyvinylpyrrolidone accounting for material total amount 1.8%, remix 8s, obtain high softening point bitumen particulate composition.Normal temperature stacks 30 days, sieves.
High softening point bitumen composition grain character in table 1 embodiment.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Softening temperature, DEG C | 152.9 | 162.7 | 175.5 | 185.4 |
| Mean particle size, mm | 106 | 80 | 62 | 80 |
| Percent of pass after sieve, % | 99.1 | 98.9 | 98.5 | 97.9 |
High softening point bitumen composition grain character in table 2 comparative example.
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Softening temperature, DEG C | 152.8 | 163.0 | 176.1 | 186.1 |
| Mean particle size, mm | 106 | 180 | 120 | 250 |
| Percent of pass after sieve, % | 50.2 | 97.2 | 97.6 | 85.2 |
Note: after sieve, percent of pass refers to: after particulate matter normal temperature stacks 30 days, is sieved with the standard sieve of same apertures when just preparing, is accounted for the percentage ratio of total mass by the granular mass of sieve aperture.The stability of this index paper examines particulate matter after storage, i.e. change of size situation.
Claims (11)
1. an Asphalt composition particle, is characterized in that: by mass percentage, comprises following component:
(1) basic asphalt: 70% ~ 94.5%;
(2) solid dispersion: 5% ~ 29.5%;
(3) coating agent: 0.1% ~ 5%;
The mean particle size of Asphalt composition particle is 10 ~ 120mm,
Wherein, basic asphalt is the mixture of oxidized bitumen and solvent deoiling pitch, and wherein oxidized bitumen accounts for 30% ~ 70% of basic asphalt quality, and solvent deoiling pitch accounts for 70% ~ 30% of basic asphalt quality.
2. Asphalt composition particle according to claim 1, is characterized in that: the mean particle size of Asphalt composition particle is 30 ~ 100mm.
3. Asphalt composition particle according to claim 1, is characterized in that: the softening temperature of basic asphalt is more than 120 DEG C.
4. Asphalt composition particle according to claim 3, is characterized in that: the softening temperature of basic asphalt is more than 150 DEG C.
5. Asphalt composition particle according to claim 1, is characterized in that: the mass percentage of basic asphalt in bituminous composition is 75% ~ 89%, and solid dispersion add-on accounts for 10% ~ 20% of bituminous composition total mass.
6. Asphalt composition particle according to claim 1 or 5, is characterized in that: solid dispersion is one or more in graphite, polynite and wilkinite.
7. Asphalt composition particle according to claim 1, is characterized in that: coating agent is one or more in water soluble resin and polyvinylpyrrolidone.
8. the preparation method of Asphalt composition particle described in a claim 1, it is characterized in that comprising following process: select basic asphalt raw material, basic asphalt raw material and solid dispersion are joined in disintegrating apparatus and carries out pre-mixing dispersion, then low temperature environment is placed in brittle to material, temperature is 0 ~-60 DEG C, and the time is 2 ~ 48 hours; After low temperature brittleness, material is pulverized in disintegrating apparatus, then adds coating agent, mixes, and namely prepares high softening point bitumen composition grain.
9. method according to claim 8, is characterized in that: be then placed in low temperature environment brittle to material, temperature is-10 ~-30 DEG C, and the time is 2 ~ 10 hours.
10. method according to claim 8 or claim 9, is characterized in that: disintegrating apparatus is high energy shear milling machine, colloidal mill or jaw crusher.
11. methods according to claim 8 or claim 9, it is characterized in that: pre-mixing jitter time is 1 ~ 10s, after low temperature brittleness, the grinding time of material is 10 ~ 40 s, and adding the mixing time after coating agent is 1 ~ 10s.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103320101B (en) * | 2013-07-11 | 2014-10-29 | 沧州科迪泥浆有限公司 | Emulsified asphalt for drilling fluids |
| CN104559233B (en) * | 2013-10-22 | 2017-04-12 | 中国石油化工股份有限公司 | Asphalt composition particle and preparation method thereof |
| CN103773029B (en) * | 2014-01-20 | 2016-03-02 | 南通东南公路工程有限公司 | A kind of acrylic resin emulsified bitumen |
| CN105542492B (en) * | 2014-11-03 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of Asphalt composition particle and preparation method |
| CN104498073A (en) * | 2015-01-07 | 2015-04-08 | 高朝阳 | Process and production line for processing natural asphalt by virtue of aid method |
| CN107383905B (en) * | 2017-07-21 | 2019-08-09 | 长沙理工大学 | A kind of high softening-point modified pitch and preparation method thereof |
| CN114772591B (en) * | 2022-05-09 | 2023-06-16 | 厦门高容纳米新材料科技有限公司 | Method and equipment for low-temperature nanocrystallization of soft material |
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| CN1616599A (en) * | 2003-11-14 | 2005-05-18 | 马孟春 | Method for producing granular pitch |
| CN101831281A (en) * | 2010-05-19 | 2010-09-15 | 濮阳市诚信钻采助剂有限公司 | High-dispersion modified asphalt powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1616599A (en) * | 2003-11-14 | 2005-05-18 | 马孟春 | Method for producing granular pitch |
| CN101831281A (en) * | 2010-05-19 | 2010-09-15 | 濮阳市诚信钻采助剂有限公司 | High-dispersion modified asphalt powder and preparation method thereof |
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