CN104559239B - Asphalt composition particles with high softening point and preparation method thereof - Google Patents
Asphalt composition particles with high softening point and preparation method thereof Download PDFInfo
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- CN104559239B CN104559239B CN201310496050.9A CN201310496050A CN104559239B CN 104559239 B CN104559239 B CN 104559239B CN 201310496050 A CN201310496050 A CN 201310496050A CN 104559239 B CN104559239 B CN 104559239B
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Abstract
The invention discloses asphalt composition particles with high softening point and a preparation method thereof. According to the composition particles, asphalt I with the high softening point is a nuclear phase, and asphalt II with the high softening point wraps the outer layer of the asphalt I; the asphalt particles comprise the following components in percentage by mass: 20-60 percent of the asphalt I with the high softening point and 40-80 percent of the asphalt II with the high softening point, wherein the softening point difference between the asphalt I with the high softening point and the asphalt II with the high softening point is 10-25 DEG C. The preparation method comprises the following steps: (1) mixing the asphalt II with the high softening point with a compatilizer to obtain mother liquor, uniformly mixing the asphalt I with the high softening point with the mother liquor in a reactor, performing blowoff treatment, and then discharging and cooling at the end of blowoff treatment to obtain an asphalt mixture with the high softening point; (2) adding the mixture obtained in the step (1), a surfactant and inorganic micro powder into crushing equipment to be mixed and crushed to prepare the asphalt particles with the high softening point. The asphalt composition particles are higher in softening point and can continuously play a role under the drilling operation condition within a wider temperature range.
Description
Technical field
The invention belongs to asphalt field is and in particular to a kind of high softening point bitumen composition grain and its preparation side
Method.
Background technology
Asphalt product is one of important additive for drilling fluid, has good anti-collapse, lubrication, emulsifying, filtrate reducing and height
Temperature stably waits comprehensive effectiveness.Asphalt product typically contains water-fast pitch particle, and has certain softening point.Work as well
When ophthalmic has sufficiently high temperature and pressure, pitch particle softening transform, and being squeezed in borehole wall microcrack, stop drilling fluid and
Filtrate is permeated from microcrack, effectively blocks stratum together with mud cake.Bitumen is that oil drilling is extremely effective anti-collapse
Agent and oil layer protective agent.With the development of Petroleum finance, drilling depth is constantly deepened, and drilling strata is more and more complicated,
The quantity of the special wells such as directional well, horizontal well gradually increases.This make drilling engineering to drilling fluid asphalt product and its
System is put forward higher requirement.Develop that high-temperature behavior is good, have good seal-off effect and the high softening point bitumen of filtration reduction (to refer to
Softening point more than 100 DEG C, especially more than 120 DEG C), to meet the needs of oil drilling engineering, have highly important
Meaning.
The preparation technology of high softening point bitumen typically adopt solvent deasphalting or air blowing oxidation technique, cn102464989a,
Cn102876344a, cn102464988a and cn102382696a etc. disclose several for the high softening point bitumen in drilling fluid
Or the preparation method of pitch particle, asphalt softening point typically more than 120 DEG C, up to 250 DEG C.
Cn102952526a discloses a kind of high softening-point emulsified asphalt water-base drilling fluid inorganic agent and preparation method thereof, institute
State additive for drilling fluid and include the Colophonium, 35～50 weight % water that 40～70% softening points are 150～240 DEG C, 0.02～2% auxiliary agent,
0.05～5 % emulsifying agent, 0.01～1% stabilizer, this additive for drilling fluid has good High Temperature High Pressure filtrate reducing function, fits
Deep-well for High Temperature High Pressure and ultra-deep well drilling.
Us7220348b1, cn102876344 a, cn102876344 a and cn102732280a also discloses several high soft
Change the production method of point Colophonium, asphaltic products softening point is all at 250 DEG C with but mainly for the production of carbon fiber product, fire proofed wood
Material binding agent and spinning field.
Existing high softening point bitumen is when being applied in the middle of drilling fluid system, single due to forming, and there is viscoelastic scope
Less, using temperature range narrower the problems such as, be difficult to persistently play a role in down-hole.Cn1046176a discloses a kind of containing in advance
About 2 parts of high softening-point Uintahites of mixing, about 1 part of low softening point Uintahite, about 1 part of causticization brown coal and a kind of strongly lipophilic are non-
The water-based drilling muds additive of ionic surface active agent.This compositions of additives can be in the temperature and pressure of wide scope
Effectively, but simple mechanical mixture is difficult to effectively play the action effect of different softening point Colophonium.Using several different softenings
Point Colophonium mechanical mixture, simple combination, is also all each to play a role, after exceeding softening point, just ineffective it is desirable to not
Reach good plugging effect in synthermal scope it is necessary to ensure the addition of every kind of softening point asphalt, further increase drip
Green grass or young crops is in the scattered difficulty of drilling fluid.
Content of the invention
For the deficiencies in the prior art, the present invention provides a kind of high softening point bitumen composition grain and preparation method thereof.
High softening point bitumen composition grain of the present invention has higher softening point, can be in the drillng operation condition of wide temperature range
Under persistently play a role.
The high softening point bitumen composition grain of the present invention, with high softening point bitumen i as nuclear phase, outer layer covers high softening-point
Colophonium ii, by mass percentage, including following component: high softening point bitumen i 20%～60%, high softening point bitumen ii 40%
～80%；The softening point difference of wherein high softening point bitumen ii and high softening point bitumen i is 10 ~ 25 DEG C.
In pitch particle of the present invention, the softening point of described high softening point bitumen i is 150 ~ 280 DEG C, preferably 180 ~ 260
DEG C, high softening point bitumen i is solid, powdery, mean diameter≤80 μm, preferably mean diameter≤60 μm, and high softening point bitumen i can
Think commercially available prod or natural Uintahite it is also possible to according to the preparation of this area routine techniquess, such as reduced pressure distillation process, solvent takes off drip
Young worker's skill, air blowing oxidation technique etc., or the combination of several technique.
In pitch particle of the present invention, the softening point of described high softening point bitumen ii is 160～300 DEG C, preferably 180～
280 DEG C, high softening point bitumen ii can be powder or graininess, and high softening point bitumen ii can be commercially available prod or natural hard
Colophonium is it is also possible to according to the preparation of this area routine techniquess, such as reduced pressure distillation process, solvent de-asphalting process, air blowing oxidation technique
Deng, or the combination of several technique.
The preparation method of the high softening point bitumen composition grain of the present invention, including following content:
(1) high softening point bitumen ii and compatilizer are mixed to get mother solution, then by high softening point bitumen i with mother solution anti-
Answer mix homogeneously in device, be passed through compressed gas from reactor bottom and carry out stripping process, compatilizer is in gas phase reacted device top
Outlet discharge, cooled can be recycled, after stripping terminates, discharging, cooling obtain high softening point bitumen mixture；
(2) mixture, surfactant and the inorganic micro powder obtaining step (1) is added in disintegrating apparatus and is mixed
Pulverize, that is, prepare high softening point bitumen granule.
In the inventive method, described compatilizer is any fraction between 100 ~ 300 DEG C for the boiling range scope, preferably 150 ~
Any fraction between 280 DEG C.
In the inventive method, the mass ratio that compatilizer is mixed with high softening point bitumen ii is 1:4 ~ 2:1, preferably 1:3 ~ 1:1.
In the inventive method, described compressed gas are one or more of air, nitrogen or noble gases.
In the inventive method, high softening point bitumen ii is 20 ~ 80 DEG C with compatilizer mixing temperature, preferably 25 ~ 75 DEG C.Mixing
Time is 5 ~ 60 minutes, preferably 10 ~ 30 minutes, and mixed process can be using common churned mechanically mode, to make the two mixing
Uniformly.
In the inventive method, described reactor is the reaction vessel with agitating function, and reactor lower part is provided with compression
Gas access, top is provided with gas outlet.
In the inventive method, the condition that described stripping is processed is: 120～300 DEG C of stripping temperature, preferably 160～280
DEG C, stripping time is 0.3～3 hour, and compressed gas inlet pressure is 0.1 ~ 0.5mpa.
In the inventive method, stripping processing procedure is preferably carried out as follows: in 120 ~ 250 DEG C of temperature, is blown
De- process 20 ~ 150 minutes, then heats to 140 ~ 300 DEG C, stripping 10 ~ 100 minutes.
In the inventive method, described stripping temperature is consistently less than the softening point of high softening point bitumen i.
In the inventive method, high softening point bitumen i is preferably dry mixed with inorganic micro powder, wherein Colophonium and inorganic micro powder
Mass ratio is 10:1 ~ 100:1, and described inorganic micro powder is one or more of graphite, montmorillonite, bentonite or brucite,
The granularity of inorganic micro powder is less than 100 μm, preferably nano grade inorganic micropowder, and above-mentioned inorganic micro powder is preferably through organically-modified inorganic
Micropowder, the such as organic modifiers such as silane coupler, titanate coupling agent.
In the inventive method, described disintegrating apparatus can be that high energy shear milling machine, colloid mill, ball mill pulverizer etc. stir
Mix or hit stirring-type disintegrating apparatus, grinding time is 10～60s, pulverize temperature and be no more than 30 DEG C, high softening point bitumen is excellent
Carry out low temperature brittleness process, low temperature brittleness treatment conditions are: temperature is 0～-60 DEG C before being selected in pulverizing, preferably -10～-30
DEG C, the time is 2～48 hours, preferably 2～10 hours.
In the inventive method, described surfactant is Dodecyl trimethyl ammonium chloride, cetyl trimethyl chlorine
Change one or more of ammonium, octadecyl trimethyl ammonium chloride, sodium lignin sulfonate or calcium lignosulfonate etc., addition accounts for
The 0.05% ~ 5% of high softening point bitumen composition grain weight, preferably 0.5% ~ 3%.
In the inventive method, described inorganic micro powder is one of graphite, montmorillonite, bentonite or brucite or several
Kind, the granularity of inorganic micro powder is less than 100 μm, preferably nano grade inorganic micropowder, and above-mentioned inorganic micro powder is preferably through organically-modified
Inorganic micro powder, addition accounts for the 1% ~ 10% of high softening point bitumen composition grain weight, and preferably 3% ~ 5%.
Phosphate ester starch, carboxymethyl starch, cationic starch, carboxymethyl can also be added as needed in the inventive method
One or more of cellulose (cmc), vinal and water solublity pva fiber.
The mean diameter of high softening point bitumen composition grain of the present invention is 50～150 μm, preferably 60～100 μm.
High softening point bitumen composition grain of the present invention in terms of oil drilling, the deep layer of particularly wide temperature
Apply in drilling fluid system.
With in prior art it is an advantage of the current invention that: high softening point bitumen composition grain of the present invention, the softening of outer layer
Point higher than 10 ~ 25 DEG C of the softening point of nuclear phase, well temperature two kinds of softening points interval and near change when, high softening point bitumen compositionss
The nuclear phase of granule first softens, but the presence due to outer layer Colophonium, will not trickle, when being extruded by external force, pitch particle
It is easily deformed, nuclear phase and outer layer viscoelastic sex differernce, be also beneficial to form fine and close mud cake, play plugging action, widened high soft
Change the Applicable temperature scope of point Asphalt composition particle.High softening point bitumen composition grain of the present invention can be according to actual need
The Colophonium of nuclear phase and outer layer is carried out with the modulation of softening point, persistently can play a role in the range of wider drilling depth.
High softening point bitumen composition grain of the present invention, compared to single or mechanical mixture high softening point bitumen mixture, has higher
Deformability, granular size can be adjusted according to actual needs, thus using the closure in different size of hole in oil reservoir, playing
Good plugging effect.
Specific embodiment
By embodiment, the present invention will be further described below, but not thereby limiting the invention, therein
Percentage composition is weight/mass percentage composition.The method of testing of softening point is carried out according to gb/t4507 method.High temperature and high pre ssure filtration is pressed
Sy/t5621 method measures.Average particle size distribution adopts laser particle analyzer to measure.
Embodiment 1
Take 100g high softening point bitumen ii(softening point to be 200 DEG C) and 70g boiling range be placed in container for 150 ~ 170 DEG C of fraction
In, 30 DEG C are stirred 35 minutes, and mother solution is obtained after being sufficiently mixed uniformly；60g high softening point bitumen i(softening point is 180 DEG C,
Mean diameter is 70 μm) mix in the reactor with mother solution, and it is passed through compressed air, gas inlet pressure is 0.2mpa, reaction
Device temperature is maintained at 140 ~ 150 DEG C, stirs 20 minutes, then heats to 170 DEG C, stirs 10 minutes, discharging, and cooling obtains high soft
Change point asphalt mixture；
High softening point bitumen mixture (the low temperature brittleness condition: -25 DEG C of temperature, the time 8 is little that 100g low temperature brittleness is processed
When), 4g brucite and 1.5g sodium lignin sulfonate, be added in high speed disintegrator, co-grinding 25s, obtain high softening-point drip
Blue or green granule, is designated as a1, and its mean diameter is 90 μm.
Embodiment 2
Take 100g high softening point bitumen ii(softening point to be 250 DEG C) and 50g kerosene be placed in container, 50 DEG C of room temperature stirs 30
Minute, mother solution is obtained after being sufficiently mixed uniformly；100g high softening point bitumen i(softening point is 220 DEG C, mean diameter is 75 μ
M) mix in the reactor with mother solution, and be passed through compressed air, gas inlet pressure is 0.25 mpa, temperature of reactor is maintained at
180 ~ 190 DEG C, stir 60 minutes, then heat to 210 DEG C, stir 10 minutes, discharging, cooling obtains high softening point bitumen mixing
Thing；
By the high softening point bitumen compositionss (brittle treatment conditions are with embodiment 1) through low temperature brittleness for the 100g, 5g graphite, 1g
Cetyl trimethylammonium bromide and 3g carboxymethyl starch are added in high speed disintegrator, and co-grinding 15s obtains high softening-point
Pitch particle, is designated as a2, and its mean diameter is 100 μm.
Embodiment 3
Take 100g high softening point bitumen ii(softening point to be 170 DEG C) and 100g gasoline be placed in container, 65 DEG C of room temperature stirs
30 minutes, mother solution is obtained after being sufficiently mixed uniformly；120g high softening point bitumen i(softening point is 145 DEG C, mean diameter is
80 μm) mix in the reactor with mother solution, and it is passed through compressed air, gas inlet pressure is 0.35mpa, and temperature of reactor keeps
At 140 DEG C, stir 60 minutes, discharging, cooling obtains high softening point bitumen mixture；
By 100g bituminous composition, 6g montmorillonite and 0.5g Cetyltrimethylammonium bromide, it is added to high speed disintegrator
In, co-grinding 30s, obtain high softening point bitumen granule, be designated as a3, its mean diameter is 80 μm.
Comparative example 1
100g high softening point bitumen i, 4g brucite and 1.5g sodium lignin sulfonate, are added in high speed disintegrator, mixing
Pulverize 25s, obtain high softening point bitumen granule, be designated as a4, its mean diameter is 90 μm.
Comparative example 2
100g high softening point bitumen ii, 5 graphite, 1g cetyl trimethylammonium bromide and 3g carboxymethyl starch are added to height
In fast pulverizer, co-grinding 20s, obtain pitch particle, be designated as a5, its mean diameter is 85 μm.
Comparative example 3
, with embodiment 3,100g high softening-point drips for the raw material of high softening point bitumen i and high softening point bitumen ii and usage ratio
The mixture of blue or green i and high softening point bitumen ii processes (brittle treatment conditions are with embodiment 1) through brittle, with 6g montmorillonite, 0.5g
Cetyltrimethylammonium bromide, is added in high speed disintegrator, and co-grinding 30s obtains pitch particle, is designated as a6, and it is put down
All particle diameter is 100 μm.
A1 ~ a6 high softening-point green grass or young crops granule is added to the base slurry preparing, high softening point bitumen particle loads account for base slurry
The 2% of weight, measure respectively under the conditions of test pressure 3.45mpa different temperatures aging after filter loss, concrete outcome is shown in Table 1.
Wherein base slurry preparation method is as follows: adds the drip of 2.75g natrium carbonicum calcinatum in 1000ml water, adds 60g calcium bentonite, high-speed stirring
Mix 20 minutes maintenance 24 hours at room temperature, obtain 6% fresh water-based slurry.
Filter loss after table 1 high softening point bitumen granule different temperatures is aging.
| Filter loss (180 DEG C)/ml | Filter loss (190 DEG C)/ml | Filter loss (200 DEG C)/ml | |
| Base is starched | 169 | 198 | 213 |
| Embodiment 1 | 34 | 18 | 25 |
| Comparative example 1 | 28 | 31 | 184 |
| Filter loss (220 DEG C)/ml | Filter loss (230 DEG C)/ml | Filter loss (250 DEG C)/ml | |
| Base is starched | 242 | 256 | 280 |
| Embodiment 2 | 205 | 188 | 20 |
| Comparative example 2 | 234 | 218 | 32 |
| Filter loss (145 DEG C)/ml | Filter loss (160 DEG C)/ml | Filter loss (170 DEG C)/ml | |
| Base is starched | 76 | 98 | 121 |
| Embodiment 3 | 45 | 25 | 21 |
| Comparative example 3 | 33 | 51 | 32 |
Note: in table, temperature is Aging Temperature, digestion time is 16 hours.
Claims (17)
1. a kind of high softening point bitumen composition grain it is characterised in that: with high softening point bitumen i as nuclear phase, outer layer covers are high
Softening point asphalt ii, by mass percentage, including following component: high softening point bitumen i 20%～60%, high softening point bitumen
Ii 40%～80%；Wherein high softening point bitumen ii is higher than the softening point of high softening point bitumen i 10 ~ 25 DEG C.
2. according to the Asphalt composition particle described in claim 1 it is characterised in that: the softening of described high softening point bitumen i
Point is 150 ~ 280 DEG C, and high softening point bitumen i is solid, powdery, mean diameter≤80 μm.
3. according to the Asphalt composition particle described in claim 1 it is characterised in that: the softening of described high softening point bitumen ii
Point is 160～300 DEG C, and high softening point bitumen ii is powder or graininess.
4. a kind of preparation method of the high softening point bitumen composition grain described in claim 1 is it is characterised in that include as follows
Then high softening point bitumen i is being reacted by content: high softening point bitumen ii is mixed to get mother solution with compatilizer by (1) with mother solution
Mix homogeneously in device, is passed through compressed gas from reactor bottom and carries out stripping process, and compatilizer goes out in gas phase reacted device top
Mouthful discharge, cooled can be recycled, after stripping terminates, discharging, cooling obtain high softening point bitumen mixture；(2) by step
(1) mixture, surfactant and the inorganic micro powder obtaining is added in disintegrating apparatus and carries out co-grinding, that is, prepare high soft
Change point Asphalt composition particle.
5. in accordance with the method for claim 4 it is characterised in that: described compatilizer be boiling range scope 100 ~ 300 DEG C it
Between any fraction.
6. in accordance with the method for claim 4 it is characterised in that: the mass ratio that compatilizer is mixed with high softening point bitumen ii is
1:4~2:1.
7. in accordance with the method for claim 4 it is characterised in that: described compressed gas are air, nitrogen or noble gases
One or more of.
8. in accordance with the method for claim 4 it is characterised in that: high softening point bitumen ii and compatilizer mixing temperature be 20 ~
80 DEG C, incorporation time is 5 ~ 60 minutes.
9. in accordance with the method for claim 4 it is characterised in that: described reactor be with agitating function reaction hold
Device, reactor lower part is provided with compressed gas entrance, and top is provided with gas outlet.
10. in accordance with the method for claim 4 it is characterised in that: the condition that described stripping is processed is: stripping temperature 120
～300 DEG C, stripping time is 0.3～3 hour, and compressed gas inlet pressure is 0.1 ~ 0.5mpa.
11. in accordance with the method for claim 4 it is characterised in that: stripping processing procedure is carried out as follows: in temperature
120 ~ 250 DEG C, carry out stripping and process 20 ~ 150 minutes, then heat to 140 ~ 300 DEG C, stripping 10 ~ 100 minutes.
12. in accordance with the method for claim 4 it is characterised in that: described stripping temperature is consistently less than high softening point bitumen i
Softening point.
13. in accordance with the method for claim 4 it is characterised in that: described disintegrating apparatus are high energy shear milling machine, colloid
One or more of mill or ball mill pulverizer, grinding time is 10～60s, pulverizes temperature and is no more than 30 DEG C.
14. in accordance with the method for claim 4 it is characterised in that: described surfactant be trimethyl chlorine
Change in ammonium, hexadecyltrimethylammonium chloride, octadecyl trimethyl ammonium chloride, sodium lignin sulfonate or calcium lignosulfonate
One or more, addition accounts for the 0.05% ~ 5% of high softening point bitumen composition grain weight, high softening point bitumen compositionss
The each constituent content sum of grain is 100%.
15. in accordance with the method for claim 4 it is characterised in that: described inorganic micro powder be graphite, montmorillonite, bentonite
One or more of or brucite, the granularity of inorganic micro powder is less than 100 μm, and addition accounts for high softening point bitumen composition grain
The 1% ~ 10% of weight, high softening point bitumen composition grain each constituent content sum is 100%.
High softening point bitumen composition grain described in 16. claim 1 it is characterised in that: high softening point bitumen compositionss
The mean diameter of grain is 50～150 μm.
Application in deep layer drilling fluid system for the high softening point bitumen composition grain described in 17. claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310496050.9A CN104559239B (en) | 2013-10-22 | 2013-10-22 | Asphalt composition particles with high softening point and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310496050.9A CN104559239B (en) | 2013-10-22 | 2013-10-22 | Asphalt composition particles with high softening point and preparation method thereof |
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| Publication Number | Publication Date |
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| CN104559239A CN104559239A (en) | 2015-04-29 |
| CN104559239B true CN104559239B (en) | 2017-01-18 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4514308A (en) * | 1983-07-29 | 1985-04-30 | Clampitt Richard L | Sulfonated asphalt |
| US5030365A (en) * | 1989-02-24 | 1991-07-09 | Chevron Research Company | Water-wettable drilling mud additives containing uintaite |
| CN102464988B (en) * | 2010-11-04 | 2014-03-05 | 中国石油化工股份有限公司 | Preparation method of high-softening-point asphalt particles for drilling fluid |
| CN102464989B (en) * | 2010-11-04 | 2014-04-02 | 中国石油化工股份有限公司 | Preparation method of high softening point asphalt |
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2013
- 2013-10-22 CN CN201310496050.9A patent/CN104559239B/en active Active
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