CN104559956B - A kind of drilling fluid high softening point bitumen particle and preparation method thereof - Google Patents
A kind of drilling fluid high softening point bitumen particle and preparation method thereof Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
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Abstract
The invention discloses a kind of drilling fluid high softening point bitumen particle, by mass percentage, including following component：High softening point bitumen composition 80wt%~95wt%, latex 5wt%~20wt%；Wherein described high softening point bitumen composition is that the softening point difference between softening point two or more mixture in the high softening point bitumen between 120 ~ 240 DEG C, the adjacent high softening point bitumen of softening point from low to high is 5 ~ 50 DEG C.High softening point bitumen particle of the present invention has higher softening point and deformability, can persistently be played a role under the conditions of the drillng operation of wide temperature range.
Description
Technical field
The invention belongs to asphalt field, and in particular to a kind of drilling fluid high softening point bitumen particle and its preparation side
Method.
Background technology
Asphalt product is one of important additive for drilling fluid, with good anti-collapse, lubrication, emulsification, filtrate reducing and height
The comprehensive effectivenesses such as temperature stabilization.Asphalt product typically contains water insoluble pitch particle, and has certain softening point.Work as well
When intraocular has sufficiently high temperature and pressure, pitch particle softening transform, and being squeezed into borehole wall microcrack, prevent drilling fluid and
Filtrate is permeated from microcrack, and stratum is effectively blocked 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 proposes higher requirement.The high softening point bitumen that high-temperature behavior is good, have good seal-off effect and filtration reduction is developed (to refer to
Softening point is more than 100 DEG C, especially more than 120 DEG C), the need for meeting oil drilling engineering, with highly important
Meaning.
The preparation technology of high softening point bitumen typically use solvent deasphalting or air blowing oxidation technique, CN102464989A,
CN102876344A, CN102464988A and CN102382696A etc. disclose several high softening point bitumens being used in drilling fluid
Or the preparation method of pitch particle, asphalt softening point is 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 including 40~70% softening points for 150~240 DEG C pitch, 35~50 weight % water, 0.02~2% auxiliary agent,
0.05~5 % emulsifying agents, 0.01~1% stabilizer, additive for drilling fluid has good HTHP filtrate reducing function, fits
Deep-well and ultra-deep well drilling for HTHP.
US7220348B1, CN102876344 A, CN102876344 A and CN102732280A also disclose several high soft
Change the production method of point pitch, asphaltic products softening point is all at 250 DEG C with but mainly for the production of carbon fiber product, fire proofed wood
Expect binding agent and spinning field.
It is single due to constituting when existing high softening point bitumen is among applied to drilling fluid system, there is viscoelastic scope
It is smaller, the problems such as temperature in use scope is narrower, it is difficult to persistently be played a role in underground.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of drilling fluid high softening point bitumen particle and its preparation side
Method.High softening point bitumen particle of the present invention have higher softening point and deformability, can wide temperature range drilling well
Persistently played a role under operating condition.
The drilling fluid high softening point bitumen particle of the present invention, by mass percentage, including following component：High softening-point
Bituminous composition 80wt%~95wt%, latex 5wt%~20wt%；Wherein described high softening point bitumen composition is that softening point exists
The mixture of two or more in high softening point bitumen between 120 ~ 240 DEG C, the adjacent height of softening point from low to high is soft
The softening point difference changed between point pitch is 5 ~ 50 DEG C, preferably 10 ~ 30 DEG C；The different high softening point bitumen of preferably 2~8 kinds of softening points
The mixture of composition；Most preferably softening point be 120 ~<150℃、150~<180 DEG C and 180 ~ 240 DEG C three kinds of high softening point bitumens
Mixture；In terms of high softening point bitumen composition weight percentage composition, the content of every kind of high softening point bitumen is not more than 90%, excellent
Choosing is not more than 70%, more preferably no more than 60%.All high softening point bitumen percentage composition sums are 100%.
High softening point bitumen composition of the present invention is solid, powdery, preferably 50~120 μm of average grain diameter, averagely grain
60~100 μm of footpath, can be commercially available prod, can also be prepared according to this area routine techniques, such as reduced pressure distillation process, solvent take off
Pitch technique, air blowing oxidation technique etc., or several techniques combination.
The present invention provides a kind of preparation method of high softening point bitumen, including following content：Asphalt stock A is with gas pre-
Mixed in mixed tank, the asphalt stock A containing gas enters oxidation reactor, fully connect with the asphalt stock B of molten condition
Touch and react jointly, after asphalt stock A is completely into reactor, is passed through gas and carries out oxidation reaction, obtain high softening-point drip
It is blue or green.High softening point bitumen obtains high softening point bitumen powder by crushing again, and grinding mode uses Freezing smashing, freezing conditions
For：Cryogenic temperature is -10 ~ -50 DEG C, and cooling time is 2 ~ 10 hours.
Described asphalt stock A is the coal tar pitch after middle temperature or high temperature distillation, and softening point is 40~90 DEG C, and carbon residue exists
More than 25wt%, accounts for 10wt%~50wt% of asphalt stock total amount.Described asphalt stock B is asphalt, including depressurizes slag
One or more of mixtures in de-oiled asphalt, mediation pitch that oil, straight asphalt, solvent de-asphalting process are obtained etc..Drip
Blue or green raw material B 25 DEG C of needle penetrations are 20~200 1/10mm, and softening point is 30~75 DEG C, account for the 50wt% of material asphalt total amount~
90wt%。
Described oxygen-containing gas is air, oxygen-enriched air or oxygen.Asphalt stock A is mixed with oxygen-containing gas in premixing tank
Close, premixing tank is closed container of the outlet with choke valve.The mixing temperature of asphalt stock A and oxygen-containing gas is 80~180 DEG C,
Blend pressure is 0.1 ~ 0.5MPa, and incorporation time is 1 ~ 60 minute.The asphalt stock A of mixing oxygen-containing gas enters oxidation reactor
Mode be spray regime.Described course of injection is the choke valve by opening premixing tank exit, makes the original rich in gas
Material A is ejected into oxidation reactor.Described oxidation reactor is batch oxidation kettle or continous way oxidizing tower.
Oxidation reaction condition is：Gas flow is 0.05~0.5m3·kg-1·h-1, oxidizing temperature is 200~320 DEG C, excellent
Elect 250 ~ 300 DEG C as, oxidization time is 3~10 hours.
In high softening point bitumen particle of the present invention, described latex is Heveatex, styrene-butadiene latex, NBR latex, neoprene
One or more in latex, polystyrene latex or polybutadiene latex, the solid content of latex is 20wt%~60wt%.
Accelerator is preferably added in high softening point bitumen particle of the present invention, on the basis of high softening point bitumen weight, is promoted
Agent addition is 1wt%~10wt%, and pitch particle each component content sum is 100%.Wherein accelerator is sulfate, quaternary ammonium salt
Or the one or more in lignosulfonates, wherein sulfate is to be modified bay alcohol radical sodium sulphate, secondary alcohol groups sodium sulphate and mix
Close the one or more in sodium alkyl sulfate etc.；Quaternary ammonium salt is DTAC, cetyl trimethyl chlorine
Change the one or more in ammonium, OTAC etc.；Lignosulfonates are sodium lignin sulfonate or lignin
Sulfoacid calcium.
In high softening point bitumen particle of the present invention, can also add as needed phosphate ester starch, CMS, sun from
One or more in sub- starch, carboxymethyl cellulose (CMC), vinal and WATER-SOLUBLE PVA FIBER, with high softening-point
On the basis of pitch weight, accelerator addition is 1wt%~10wt%, and pitch particle each component content sum is 100%.
The preparation method of the drilling fluid high softening point bitumen particle of the present invention, including following content：Latex is uniformly sprayed
It is spread across on high softening point bitumen composition, stands infiltration a period of time, through vacuum freeze drying, obtain drilling fluid high softening-point
Pitch particle.
In the inventive method, the mass ratio of high softening point bitumen composition and latex is 5：1~1：1.
In the inventive method, sprinkling latex can use the equipment with spraying function, such as watering can, spraying machine, sprayer
Deng material being stirred or mixed and stirred during sprinkling, latex is dispersed in pitch particle surface.
In the inventive method, described standing time of penetration is 0.5 ~ 2 hour, is stood at normal temperatures.
In the inventive method, the condition of vacuum freeze drying is：Drying temperature be -10~-50 DEG C, preferably -20 ~ -40 DEG C,
Cooling time 5~24 hours, preferably 10 ~ 18 hours.Need to carry out pre-freeze before vacuum freeze drying, pre-freezing temperature is -30 ~ -50 DEG C,
The pre-freeze time is 1 ~ 4 hour.
High softening point bitumen particle of the present invention is particularly applied in terms of oil drilling in deep layer drilling fluid system.
With in the prior art the advantage of the invention is that：
（1）Suitable raw material is selected when preparing high softening point bitumen, that is, have selected a part of asphalt, have selected again
Part of coal pitch.One side coal tar pitch is after certain temperature is heated to, and viscosity can become smaller, advantageously form injection stream
Body, is fully contacted with the raw material in reactor.This fluid is rich in more oxygen, and oxidation reaction can be made to be more easy to occur and enter
OK.On the other hand, coal tar pitch be coal tar after middle temperature or high temperature distillation obtained by residue, mainly by polycyclic aromatic hydrocarbon and
Its derivative and heterocyclic compound composition.Compared with petroleum-type residual oil or pitch, with higher oxidation activity and instead
Should be from emission capacity.Therefore in whole course of reaction, less heat energy only need to be provided, just can be with the shorter reaction time
Product softening point is effectively improved, without adding other additives such as catalyst.Greatly reduce production cost.
（2）Although it is good that asphalt glues warm nature, it is difficult to be ground into tiny particle, and the same terms under normal temperature
Under, softening point rising is more slow compared with coal tar pitch raw material, if being not added with catalyst hardly results in high softening point bitumen；Coal is dripped
Blue brittleness is big, is easily crushed under normal temperature, but the deformability of particle is poor, is difficult arbitrarily to be embedded into the duct of crack in use
Go, filtrate reducing effect is relatively poor.It from two kinds of raw material mixed oxidizations, can learn from other's strong points to offset one's weaknesses, make the combination property of product significantly
Improve.
（3）The method compounded using several softening point grade bitumens, can adapt to broader temperature range；While glue
Breast has preferable affinity with pitch particle, can be uniformly adhered to the surface of pitch, add the deformable energy of particle
Power, that is, add its viscoelastic and use scope.On the other hand, in drillng operation, particle in the presence of pressure and other external force,
Small part latex can form film between the borehole wall and mud cake, improve the compactness of mud cake, serve reduction well high
The effect of the high filter pressing loss of temperature.
Embodiment
The present invention will be further described by embodiment below, but it is not thereby limiting the invention, it is therein
Percentage composition is weight/mass percentage composition.The method of testing of softening point is carried out according to GB/T4507 methods.High temperature and high pre ssure filtration is pressed
SY/T5621 methods are determined.
Embodiment 1
It is 61 1/10mm by 25 DEG C of needle penetrations, softening point is 46.3 DEG C of decompression residuum, accounts for total amount（Decompression residuum and coal
Pitch gross mass, similarly hereinafter）80.0%, be placed in stills for air blowing and be heated to 140 DEG C of molten states.Softening point is added in premixing tank is
65.4 DEG C, the coal tar pitch for accounting for total amount 20.0% is heated to 160 DEG C, is passed through air and keeps pressure inside the tank to be 0.12MPa, time 20
Minute.Choke valve is opened, coal tar pitch liquid is gradually injected in stills for air blowing, after after complete spray into, adjustment air mass flow is 0.2
m3·kg-1·h-1, air blowing oxidation is carried out, oxidizing condition and product property are shown in Table 1.
By the chilled high softening point bitumens of 100g（Freezing conditions：- 25 DEG C of temperature, 8 hours time）It is added to high speed powder
In broken machine, co-grinding 25s obtains high softening point bitumen powder, and average grain diameter is 85 μm.
Embodiment 2
It is 82 1/10mm by 25 DEG C of needle penetrations, softening point is 45.7 DEG C of decompression residuum, accounts for the 75.0% of total amount（m）, put
130 DEG C of molten states are heated in stills for air blowing.It is 49.3 DEG C that softening point is added in premixing tank, accounts for total amount 25.0%（m）Coal drip
Green grass or young crops is heated to 150 DEG C, is passed through air and keeps pressure inside the tank to be 0.18MPa, 35 minutes time.Choke valve is opened, by coal tar pitch
Liquid is gradually injected in stills for air blowing, and after after complete spray into, adjustment air mass flow is 0.20 m3·kg-1·h-1, carry out air blowing oxygen
Change, oxidizing condition and product property are shown in Table 1.
By the chilled high softening point bitumens of 100g（Freezing conditions：- 30 DEG C of temperature, 10 hours time）It is added to high speed powder
In broken machine, co-grinding 20s obtains high softening point bitumen powder, and average grain diameter is 70 μm.
Embodiment 3
It is 43 1/10mm by 25 DEG C of needle penetrations, softening point is 48.5 DEG C of decompression residuum, accounts for the 65.0% of total amount（m）, put
150 DEG C of molten states are heated in stills for air blowing.It is 56.2 DEG C that softening point is added in premixing tank, accounts for total amount 35.0%（m）Coal drip
Green grass or young crops is heated to 160 DEG C, is passed through air and keeps pressure inside the tank to be 0.25MPa, 50 minutes time.Choke valve is opened, by coal tar pitch
Liquid is gradually injected in stills for air blowing, and after after complete spray into, adjustment air mass flow is 0.22 m3·kg-1·h-1, carry out air blowing oxygen
Change, oxidizing condition and product property are shown in Table 1.
By the chilled high softening point bitumens of 100g（Freezing conditions：- 40 DEG C of temperature, 6 hours time）It is added to high speed powder
In broken machine, co-grinding 30s obtains high softening point bitumen powder, and average grain diameter is 50 μm.
Embodiment 4
It is 43 1/10mm by 25 DEG C of needle penetrations, softening point is 48.5 DEG C of decompression residuum, accounts for the 60.0% of total amount, is placed in oxygen
Change in kettle and be heated to 150 DEG C of molten states.It is 82.6 DEG C that softening point is added in premixing tank, accounts for total amount 40.0%（m）Coal tar pitch add
Heat is passed through air and keeps pressure inside the tank to be 0.25MPa, 50 minutes time to 160 DEG C.Choke valve is opened, by coal tar pitch liquid
Gradually it is injected in stills for air blowing, after after complete spray into, adjustment air mass flow is 0.28 m3·kg-1·h-1, air blowing oxidation is carried out,
Oxidizing condition and product property are shown in Table 1.
By the chilled high softening point bitumens of 100g（Freezing conditions：- 35 DEG C of temperature, 8 hours time）It is added to high speed powder
In broken machine, co-grinding 15s obtains high softening point bitumen powder, and average grain diameter is 70 μm.
The high softening point bitumen preparation condition of table 1 and product property.
Embodiment 5
（1）By mass, 100g high softening point bitumens are taken（Including：The pitch 35% obtained in embodiment 1, embodiment
The pitch 30% obtained in the pitch 35% obtained in 2, embodiment 4）Mixed.On the basis of high softening point bitumen quality, plus
Enter 4% CMS, 3% cationic starch, 3.5% vinal and 0.5% OTAC, in normal temperature
Lower stirring 30 seconds, obtains high softening point bitumen composition.
（2）Take 40g styrene-butadiene latexes（Solid content 40%）It is placed in watering can, latex is uniformly sprayed onto obtained by above-mentioned experiment
On pitch particle, stirred in sprinkling.After sprinkling terminates, normal temperature stands 40 minutes, carries out vacuum freeze drying（Pre-freezing temperature
For -40 DEG C, the pre-freeze time is 2 hours, -20 DEG C of drying temperature, and drying time is 10 hours）Drilling fluid is obtained to be dripped with high softening-point
Blue or green particle.
Embodiment 6
By mass, 100g high softening point bitumens are taken（Including：In the pitch 20% obtained in embodiment 1, embodiment 2
The pitch 25% obtained in the pitch 30% obtained in obtained pitch 25%, embodiment 3, embodiment 4）Mixed.By height softening
On the basis of point asphalt quality, 5% CMS, 4.5% cationic starch and 0.3% hexadecyltrimethylammonium chloride are added.
25s is stirred under normal temperature, high softening point bitumen composition is obtained.
Take 50g polychloroprene latexs（Solid content 30%）It is placed in watering can, latex is uniformly sprayed onto to the pitch obtained by above-mentioned experiment
On particle, stirred in sprinkling.After sprinkling terminates, normal temperature stands 60 minutes.5.0% sodium lignin sulfonate is added, is well mixed,
Carry out vacuum freeze drying（- 35 DEG C of pre-freezing temperature, 3 hours pre-freeze time；- 20 DEG C of drying temperature, 12 hours drying times）, obtain
To drilling fluid high softening point bitumen particle.
Embodiment 7
By mass, 100g high softening point bitumens are taken（Including：In the pitch 10% obtained in embodiment 1, embodiment 3
The pitch 10% obtained in obtained pitch 80%, embodiment 4）Mixed.On the basis of high softening point bitumen, 4% carboxylic first is added
Base starch, 5% WATER-SOLUBLE PVA FIBER and 0.2% OTAC.35s is stirred at normal temperatures, obtains high softening-point
Bituminous composition.
Take 80g NBR latexes（Solid content 30%）It is placed in watering can, latex is uniformly sprayed onto to the pitch obtained by above-mentioned experiment
On particle, stirred in sprinkling.After sprinkling terminates, normal temperature stands 80 minutes.Carry out vacuum freeze drying（- 40 DEG C of pre-freezing temperature,
3 hours pre-freeze time；- 25 DEG C of drying temperature, 15 hours drying times）, obtain drilling fluid high softening point bitumen particle.
The high softening point bitumen particle obtained in above example is added in the base slurry prepared, addition is starched by base
The percentages of quality, carry out drilling liquid performance evaluating.Determine different temperatures aging respectively under the conditions of test pressure 3.45MPa
Filter loss afterwards, concrete outcome is shown in Table 2.Wherein pitch 1 ~ 8 is the bituminous composition obtained in embodiment 1 ~ 7 and comparative example 1
Grain.As can be seen that drilling fluid of the present invention is improved with high softening point bitumen particle under the performance of drilling fluid, particularly high temperature
Performance, can persistently be played a role within the scope of wider temperature, serve well closure, filtrate reducing effect, Ke Yi
Continuously used under deep-well.
Comparative example 1
Step（1）Be the same as Example 5, step is not passed through simply（2）Processing.
Performance after the pitch particle different temperatures aging of table 2.
| High temperature and high pre ssure filtration（100 ℃）/mL | High temperature and high pre ssure filtration（130 ℃）/ mL | High temperature and high pre ssure filtration（150 ℃）/ mL | High temperature and high pre ssure filtration（180 ℃）/ mL | High temperature and high pre ssure filtration（200 ℃）/ mL | |
| Base is starched | 34.0 | 51.2 | 94.0 | 142.6 | 206 |
| Base slurry+2% Pitch 1 | 29.2 | 43.5 | 19.5 | 97.8 | 189.7 |
| Base slurry+2% Pitch 2 | 20.2 | 21.6 | 58.2 | 112.5 | 199.6 |
| Base slurry+2% Pitch 3 | 32.1 | 46.6 | 23.5 | 28.8 | 87.4 |
| Base slurry+2% Pitch 4 | 31.8 | 49.6 | 60.5 | 20.1 | 30.5 |
| Base slurry+2% Pitch 5 | 25.0 | 16.2 | 19.4 | 60.6 | 24.3 |
| Base slurry+2% Pitch 6 | 23.6 | 15.3 | 18.2 | 19.5 | 24.6 |
| Base slurry+2% Pitch 7 | 28.5 | 23.2 | 17.3 | 16.2 | 29.7 |
| Base slurry+2% Pitch 8 | 29.0 | 20.9 | 24.7 | 73.3 | 29.9 |
Note：Temperature is Aging Temperature in table, and digestion time is 16 hours.
Claims (18)
1. a kind of drilling fluid high softening point bitumen particle, it is characterised in that：By mass percentage, including following component：It is high
Softening point asphalt composition 80wt%~95wt%, latex 5wt%~20wt%；Wherein described high softening point bitumen composition is soft
Change o'clock two or more mixture, the phase of softening point from low to high in the high softening point bitumen between 120 ~ 240 DEG C
Softening point difference between adjacent high softening point bitumen is 5 ~ 50 DEG C；Described latex is Heveatex, styrene-butadiene latex, NBR latex, chlorine
One or more in fourth latex, polystyrene latex or polybutadiene latex, the solid content of latex is 20wt%~60wt%.
2. according to the pitch particle described in claim 1, it is characterised in that：High softening point bitumen composition is 2~8 kinds of softening points
The mixture of different high softening point bitumen compositions.
3. according to the pitch particle described in claim 1, it is characterised in that：High softening point bitumen composition be softening point be 120 ~
<150℃、150~<The mixture of 180 DEG C and 180 ~ 240 DEG C three kinds of high softening point bitumens；Contained with oxidized asphalt particle weight percentage
Gauge, the content of every kind of high softening point bitumen is not more than 90%.
4. according to the pitch particle described in claim 1, it is characterised in that：Described high softening point bitumen composition is solid powder
Shape, 50~120 μm of average grain diameter.
5. according to the pitch particle described in claim 1, it is characterised in that：The preparation method of high softening point bitumen, including it is as follows
Content：Asphalt stock A is mixed with gas in premixing tank, and the asphalt stock A of oxygen-containing gas enters oxidation reactor, with molten
The asphalt stock B of state fully contact and react jointly, after asphalt stock A is completely into reactor, is passed through gas progress
Oxidation reaction, obtains high softening point bitumen.
6. according to the pitch particle described in claim 5, it is characterised in that：Described asphalt stock A is to be steamed through middle temperature or high temperature
Coal tar pitch after evaporating, softening point is 40~90 DEG C, and carbon residue accounts for 10wt%~50wt% of asphalt stock total amount in more than 25wt%.
7. according to the pitch particle described in claim 5, it is characterised in that：Described asphalt stock B decompression residuum, straight run drip
De-oiled asphalt that blue or green, solvent de-asphalting process is obtained, the one or more of mixtures reconciled in pitch, the 25 of asphalt stock B
DEG C needle penetration is 20~200 1/10mm, and softening point is 30~75 DEG C, accounts for 50wt%~90wt% of material asphalt total amount.
8. according to the pitch particle described in claim 5, it is characterised in that：Described oxygen-containing gas is air or oxygen.
9. according to the pitch particle described in claim 5, it is characterised in that：The mixing temperature of asphalt stock A and oxygen-containing gas is
80~180 DEG C, blend pressure is 0.1 ~ 0.5MPa, and incorporation time is 1 ~ 60 minute.
10. according to the pitch particle described in claim 5, it is characterised in that：The asphalt stock A for mixing oxygen-containing gas enters oxidation
The mode of reactor is spray regime.
11. according to the pitch particle described in claim 5, it is characterised in that：Described oxidation reaction condition is：Gas flow is
0.05~0.5m3·kg-1·h-1, oxidizing temperature is 200~320 DEG C, and oxidization time is 3~10 hours.
12. according to the pitch particle described in claim 1, it is characterised in that：Accelerator is added in high softening point bitumen particle, with
On the basis of high softening point bitumen weight, accelerator addition is 1wt%~10wt%；Wherein accelerator be sulfate, quaternary ammonium salt or
One or more in lignosulfonates.
13. according to the pitch particle described in claim 1, it is characterised in that：Phosphate is added in high softening point bitumen particle to form sediment
One or more in powder, CMS, cationic starch, carboxymethyl cellulose and WATER-SOLUBLE PVA FIBER, with high softening-point
On the basis of pitch weight, accelerator addition is 1wt%~10wt%.
14. the preparation method of the drilling fluid high softening point bitumen particle described in a kind of claim 1, it is characterised in that including such as
Lower content：Latex is uniformly sprayed onto on high softening point bitumen composition, infiltration a period of time is stood, through vacuum freeze drying,
Obtain drilling fluid high softening point bitumen particle.
15. in accordance with the method for claim 14, it is characterised in that：The mass ratio of high softening point bitumen composition and latex is
5：1~1：1.
16. in accordance with the method for claim 14, it is characterised in that：Described standing time of penetration is 0.5 ~ 2 hour.
17. in accordance with the method for claim 14, it is characterised in that：The condition of vacuum freeze drying is：Drying temperature is -10
~-50 DEG C, cooling time 5~24 hours.
18. application of the high softening point bitumen particle in oil drilling described in a kind of claim 1.
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| CN106221718B (en) * | 2016-08-30 | 2018-09-25 | 中国科学院山西煤炭化学研究所 | A kind of preparation method of high softening point bitumen |
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|---|---|---|---|---|
| CN100513508C (en) * | 2006-06-23 | 2009-07-15 | 中国石油天然气股份有限公司 | Oil-soluble cationic broad-spectrum temporary plugging agent for drilling fluid |
| CN102516960B (en) * | 2011-10-17 | 2013-10-16 | 中国石油天然气股份有限公司 | Micro-suspension self-selection plugging and conditioning agent and application method thereof |
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2013
- 2013-10-22 CN CN201310497207.XA patent/CN104559956B/en active Active
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| CN104559956A (en) | 2015-04-29 |
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