CN103804926B - A kind of Asphalt composition particle and preparation method thereof - Google Patents
A kind of Asphalt composition particle and preparation method thereof Download PDFInfo
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- CN103804926B CN103804926B CN201210439805.7A CN201210439805A CN103804926B CN 103804926 B CN103804926 B CN 103804926B CN 201210439805 A CN201210439805 A CN 201210439805A CN 103804926 B CN103804926 B CN 103804926B
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Abstract
The invention discloses a kind of Asphalt composition particle and preparation method thereof.This Asphalt composition particle, weight percentage comprises following component: high softening point bitumen 80wt% ~ 95wt%, treated starch and/or water soluble fibre 4.9wt% ~ 15wt%, promotor 0.1wt% ~ 5wt%; Wherein high softening point bitumen is softening temperature at the pitch of 120 ~ 220 DEG C, and promotor is one or more in vitriol, quaternary ammonium salt or sulfonated lignin.Preparation method comprises following content: high softening point bitumen, treated starch and/or water soluble fibre and promotor are carried out co-grinding, obtains Asphalt composition particle.Asphalt composition particle of the present invention has higher softening temperature, and high-temperature behavior is excellent, and can use under the drilling operation condition of high temperature, preparation method is simple, easy to operate.
Description
Technical field
The present invention relates to a kind of Asphalt composition particle, relate in particular to a kind of oil field welldrilling high softening point bitumen composition grain and preparation method thereof.
Background technology
Along with the development of petroleum industry, drilling applications constantly expands, and the application of pitch class plugging agent in oil drilling more and more comes into one's own.Pitch class plugging agent generally containing water-fast pitch particle, and has certain softening temperature.When there being sufficiently high temperature and pressure in well, pitch particle softening transform, and be squeezed in borehole wall microfracture, stops drilling fluid and filtrate to be permeated from microfracture, shutoff stratum effectively together with mud cake.Bitumen is the extremely effective anti-sloughing agent of petroleum drilling and oil layer protective agent.In drilling operation for deep-seated oil gas field, general softening point asphalt can cannot meet the high-temperature service requirement under deep-well because of overbating or trickle.High softening point bitumen (softening temperature more than 100 DEG C, the pitch especially more than 120 DEG C) then can meet the requirement of deep layer drilling well because of its outstanding high-temperature resistance.
High softening point bitumen production technique mainly adopts solvent de-asphalting process or oxidizing process.According to existing solvent de-asphalting process, high softening point bitumen be expected, heavier solvent will be adopted.For remove pitch mutually in solvent, need be heated to higher temperature, very easily cause the problems such as furnace coking, and energy consumption is very large.In addition, even if the viscosity of high softening point bitumen is still very large at a higher temperature, production discharging is also more difficult, therefore current solvent de-asphalting process not very suitable for producing high softening point bitumen.
The advantages such as compared with solvent de-asphalting process, oxidizing process has less investment, and technique is simple, easy to operate, can yet be regarded as and produce the comparatively ideal process means of high softening point bitumen.But in traditional oxidized bitumen technological operation, pressurized air imports in raw material by an air distribution ring with very thin nozzle, and this causes the adverse consequences of coking by causing overreact near air distribution ring.Not only cause efficiency low, and reaction is also very uneven.In fact, reaction only occurs bottom oxidizing tower.
CN1415699A discloses a kind of production method of oxidized bitumen, first adopts static mixer by air and pitch mixing, makes air with small air bubbles dispersion in asphalt stock, then enter oxidation unit and carry out oxidizing reaction.When production ordinary road pitch and building asphalt, the method can improve oxidation efficiency to a certain extent.But for production high softening point bitumen, this kind of technique also exists obvious deficiency.Because the mixing temperature at static mixer Raw and air is oxidizing temperature, and produce high softening point bitumen and will carry out at a higher temperature.Mixing under such temperature conditions, can only have the air bubbles dispersion of seldom amount in raw material, therefore will be very limited to the degree improving oxidation efficiency.Along with the prolongation in reaction times and the rising of temperature of reaction, coking phenomenon is still inevitable.
In order in lower temperature of reaction with in the shorter reaction times, obtain the pitch that softening temperature is high, usually adopt the method for catalyzed oxidation, namely add a certain amount of catalyzer in the reaction, improve speed of response.CN102464989A discloses a kind of method adopting premixed catalyzed oxidation to produce high softening point bitumen.The method increase oxidation efficiency, reduce oxidization time and temperature, but need to add a certain amount of catalyzer.Not only increase cost, and the catalyzer adopted is acidic substance, long-time production can cause the corrosion of equipment, shortens the problems such as production cycle.
When high softening point bitumen uses in drilling fluid, require with minimum Granular composite in mud system, so both can ensure that pitch is uniformly dispersed, can avoid again being agglomerated into large 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.Due to the physical property that it is special, 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, CN1051957A, CN101108963A, CN1715334A and CN101311243A in succession disclose to adopt and in pitch, add calcium carbonate or other inert solid auxiliary material solve the problem that pitch is difficult to be ground into fine particle.But this method can cause the reduction of effective constituent in asphalt powder, and owing to introducing other component, in use may cause the destruction of mud system in addition.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of Asphalt composition particle and preparation method thereof.Asphalt composition particle of the present invention has higher softening temperature, and high-temperature behavior is excellent, is applicable to deep layer drilling operation.Preparation method of the present invention is simple, easy to operate, reaction efficiency is high.
Asphalt composition particle of the present invention, weight percentage comprises following component: high softening point bitumen 80wt% ~ 95wt%, treated starch and/or water soluble fibre 4.9wt% ~ 15wt%, promotor 0.1wt% ~ 5wt%; Asphalt composition particle median size≤100mm.Wherein high softening point bitumen is softening temperature at the pitch of 120 DEG C ~ 220 DEG C.
Treated starch of the present invention is one or more in phosphate ester starch, carboxymethyl starch or cationic starch etc.
Water soluble fibre of the present invention is one or more in carboxymethyl cellulose (CMC), polyvinyl alcohol fiber and WATER-SOLUBLE PVA FIBER.
Promotor of the present invention is one or more in vitriol, quaternary ammonium salt or sulfonated lignin, and wherein vitriol is one or more of modification bay alcohol radical sodium sulfate, secondary alcohol groups sodium sulfate and mixed fatty alcohol sodium sulfate etc.; Quaternary ammonium salt is one or more of Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride etc.; Sulfonated lignin are sodium lignosulfonate or calcium lignin sulphonate.
The preparation method of Asphalt composition particle of the present invention, comprises following content: high softening point bitumen, treated starch and/water soluble fibre and promotor are carried out co-grinding, obtains Asphalt composition particle.
In the inventive method, disintegrating apparatus can be stirring-type or impact type mechanical crusher.Pulverizing temperature is normal temperature, grinding time 10 ~ 60 seconds.
In the inventive method, high softening point bitumen can be prepared by existing method, preferably by the following method preparation of the present invention.
The preparation method of high softening point bitumen of the present invention, comprise following content: asphalt stock A mixes with oxygen-containing gas, the asphalt stock A of mixing oxygen-containing gas enters oxidation reactor, carry out fully contacting with the asphalt stock B of molten state and jointly react, then pass into oxygen-containing gas and carry out oxidizing reaction, obtain high softening point bitumen.
Wherein asphalt stock A is the coal-tar pitch after middle temperature or pyrogenic distillation, and softening temperature is 40 ~ 90 DEG C, and carbon residue, at more than 25wt%, accounts for the 10wt% ~ 50wt% of asphalt stock total amount.Asphalt stock B is petroleum pitch, comprises vacuum residuum, de-oiled asphalt that straight-run pitch, solvent de-asphalting process obtain, the mixture of one or more that is in harmonious proportion in pitch etc.25 DEG C of penetration degrees of asphalt stock B are 20 ~ 2001/10mm, and softening temperature is 30 ~ 75 DEG C, accounts for the 50wt% ~ 90wt% of material asphalt total amount.
Described oxygen-containing gas is air, oxygen-rich air or oxygen.
Asphalt stock A mixes in premixing tank with oxygen-containing gas, and premixing tank is the encloses container of outlet with throttling valve.The mixing temperature of asphalt stock A and oxygen-containing gas is 80 ~ 180 DEG C, and blend pressure is 0.1 ~ 0.5MPa, and mixing time is 1 ~ 60 minute.
The mode that the asphalt stock A of mixing oxygen-containing gas enters oxidation reactor is spray regime.
Described course of injection is the throttling valve by opening premixing tank exit, and the raw material A being rich in gas is ejected in oxidation reactor.
Described oxidation reactor is batch oxidation still or continous way oxidizing tower.Oxidation reaction condition is: gas flow is 0.05 ~ 0.5m
3× kg
-1× h
-1, oxidizing temperature is 200 ~ 320 DEG C, and be preferably 250 ~ 300 DEG C, oxidization time is 3 ~ 10 hours.
Asphalt composition particle of the present invention, in oil drilling, is particularly applied in deep layer drilling fluid system.
The present invention compared with prior art, has the following advantages:
(1) selecting suitable raw material when preparing high softening point bitumen, namely have selected a part of petroleum pitch, have selected again part of coal pitch.Coal-tar pitch is after being heated to certain temperature on the one hand, and viscosity can become less, is conducive to being formed spraying fluid, fully contacts with the raw material in reactor.This fluid is rich in more oxygen, oxidizing reaction can be made more easily to occur and carry out.On the other hand, coal-tar pitch is the residue that coal tar obtains after middle temperature or pyrogenic distillation, primarily of Polycyclic aromatic hydrocarbons and Derivatives and heterogeneous ring compound composition.Compared with petroleum-type residual oil or pitch, there is higher oxidation activity and react from emission capacity.Therefore, in whole reaction process, only need provide less heat energy, within the shorter reaction times, just can effectively improve product softening temperature, and without the need to adding other additives such as catalyzer.Greatly reduce production cost.
(2) although the sticky warm nature of petroleum pitch is good, under normal temperature, be not easily ground into tiny particle, and under the same terms, softening temperature rises compared with coal tar pitch raw material, is difficult to obtain high softening point bitumen if do not add catalyzer comparatively slow; Coal-tar pitch fragility is large, and easily pulverize under normal temperature, but the deformability of particle is poor, be in use not easily embedded into arbitrarily in duct, crack and go, filtrate reducing effect is relatively poor.Select two kinds of raw material mixed oxidizations, can learn from other's strong points to offset one's weaknesses, the over-all properties of product is improved greatly.
(3) the various additives added, serve respective effect.As treated starch and water soluble fibre both can serve as dispersion agent when pulverizing, preventing the pitch particle after pulverizing from again boning, its various composition can be made again in the middle of drilling fluid system to be conducive to forming colloidal form dispersion.The promotor added is and promotes dispersion agent in water, and pitch particle can be impelled dispersed in water.The rheological of drilling fluid can be improved, improve the compactness of mud cake, thus improve the performance such as leak stopping, filtrate reducing of system.
Embodiment
To be further described the present invention by embodiment below, but not thereby limiting the invention, and percentage composition is wherein mass percentage.The testing method of softening temperature is carried out according to GB/T4507 method.High temperature and high pre ssure filtration is pressed SY/T5621 method and is measured.
Embodiment 1
Be 611/10mm by 25 DEG C of penetration degrees, softening temperature is the vacuum residuum of 46.3 DEG C, accounts for 80.0% of total amount (vacuum residuum and coal-tar pitch total mass, lower with), is placed in stills for air blowing and is heated to 140 DEG C of molten states.In premixing tank, add softening temperature is 65.4 DEG C, and the coal-tar pitch accounting for total amount 20.0% is heated to 160 DEG C, passes into air and keeps tank internal pressure to be 0.12MPa, 20 minutes time.Open throttling valve, be injected to gradually in stills for air blowing by coal-tar pitch liquid, after spraying into completely, adjustment air flow quantity is 0.2m
3× kg
-1× h
-1, carry out air blowing oxidation, oxidizing condition and product property are in table 1.
100g high softening point bitumen is placed in micromill, is benchmark by high softening point bitumen composition grain quality, adds 5% carboxymethyl starch, 4.5% cationic starch and 0.5% palmityl trimethyl ammonium chloride.Stir 25 seconds at normal temperatures, obtain high softening point bitumen composition grain.
Embodiment 2
Be 821/10mm by 25 DEG C of penetration degrees, softening temperature is the vacuum residuum of 45.7 DEG C, accounts for 75.0% of total amount, is placed in stills for air blowing and is heated to 130 DEG C of molten states.In premixing tank, add softening temperature is 49.3 DEG C, and the coal-tar pitch accounting for total amount 25.0% is heated to 150 DEG C, passes into air and keeps tank internal pressure to be 0.18MPa, 35 minutes time.Open throttling valve, be injected to gradually in stills for air blowing by coal-tar pitch liquid, after spraying into completely, adjustment air flow quantity is 0.20m
3× kg
-1× h
-1, carry out air blowing oxidation, oxidizing condition and product property are in table 1.
100g high softening point bitumen is placed in micromill, is benchmark by high softening point bitumen composition grain quality, adds 7% carboxymethyl starch, 2.6% phosphate ester starch and 0.4% mixed fatty alcohol sodium sulfate.Stir 20 seconds at normal temperatures, obtain high softening point bitumen composition grain.
Embodiment 3
Be 431/10mm by 25 DEG C of penetration degrees, softening temperature is the vacuum residuum of 48.5 DEG C, accounts for 65.0% of total amount, is placed in stills for air blowing and is heated to 150 DEG C of molten states.In premixing tank, add softening temperature is 56.2 DEG C, and the coal-tar pitch accounting for total amount 35.0% is heated to 160 DEG C, passes into air and keeps tank internal pressure to be 0.25MPa, 50 minutes time.Open throttling valve, be injected to gradually in stills for air blowing by coal-tar pitch liquid, after spraying into completely, adjustment air flow quantity is 0.22m
3× kg
-1× h
-1, carry out air blowing oxidation, oxidizing condition and product property are in table 1.
100g high softening point bitumen is placed in micromill, is benchmark by high softening point bitumen composition grain quality, adds 4.5% cationic starch, 4.5% WATER-SOLUBLE PVA FIBER and 0.1% sodium lignosulfonate.Stir 30 seconds at normal temperatures, obtain high softening point bitumen composition grain.
Embodiment 4
Be 431/10mm by 25 DEG C of penetration degrees, softening temperature is the vacuum residuum of 48.5 DEG C, accounts for 60.0% of total amount, is placed in stills for air blowing and is heated to 150 DEG C of molten states.In premixing tank, add softening temperature is 82.6 DEG C, and the coal-tar pitch accounting for total amount 40.0% is heated to 160 DEG C, passes into air and keeps tank internal pressure to be 0.25MPa, 50 minutes time.Open throttling valve, be injected to gradually in stills for air blowing by coal-tar pitch liquid, after spraying into completely, adjustment air flow quantity is 0.28m
3× kg
-1× h
-1, carry out air blowing oxidation, oxidizing condition and product property are in table 1.
100g high softening point bitumen is placed in micromill, be benchmark by high softening point bitumen composition grain quality, add 6.5% cationic starch, 4.0% carboxymethyl starch and 0.1% sodium lignosulfonate, stir 20 seconds at normal temperatures, obtain high softening point bitumen composition grain.
Table 1 high softening point bitumen preparation condition and product property.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Oxidizing temperature, DEG C | 260-290 | 250-280 | 270-300 | 270-300 |
| Oxidization time, min | 420 | 420 | 480 | 560 |
| Air quantity, m 3×kg -1×h -1 | 0.2 | 0.2 | 0.22 | 0.28 |
| Heating power, kw | 1.5 | 1.8 | 1.5 | 1.5 |
| Softening temperature, DEG C | 147.9 | 123.3 | 168.4 | 186.6 |
| Mean particle size, mm | ＜100 | ＜100 | ＜100 | ＜100 |
The high softening point bitumen particle obtained in above embodiment is joined in the base slurry prepared, add-on presses the percentages of base slurry quality, carry out drilling liquid performance evaluating, measure respectively under test pressure 3.45MPa condition differing temps aging after filter loss, concrete outcome is in table 2.Its medium pitch 1 is the Asphalt composition particle obtained in embodiment 1, the like.Can find out, Asphalt composition particle of the present invention improves the performance under the use properties of drilling fluid, particularly high temperature, serves good shutoff, filtrate reducing effect, can use under deep-well.
Performance after table 2 pitch particle differing temps is aging.
| High temperature and high pre ssure filtration (100 DEG C)/mL | High temperature and high pre ssure filtration (130 DEG C)/mL | High temperature and high pre ssure filtration (150 DEG C)/mL | High temperature and high pre ssure filtration (180 DEG C)/mL | High temperature and high pre ssure filtration (200 DEG C)/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 |
Note: in table, temperature is Aging Temperature, and digestion time is 16 hours.
Claims (15)
1. an Asphalt composition particle, is characterized in that: weight percentage comprises following component: high softening point bitumen 80wt% ~ 95wt%, treated starch and/or water soluble fibre 4.9wt% ~ 15wt%, promotor 0.1wt% ~ 5wt%; Wherein high softening point bitumen is softening temperature at the pitch of 120 ~ 220 DEG C, and promotor is one or more in vitriol, quaternary ammonium salt or sulfonated lignin; The preparation method of high softening point bitumen wherein, comprise following content: asphalt stock A mixes with oxygen-containing gas, the asphalt stock A of mixing oxygen-containing gas enters oxidation reactor, carry out fully contacting with the asphalt stock B of molten state and jointly react, then pass into oxygen-containing gas and carry out oxidizing reaction, obtain high softening point bitumen; Asphalt stock A is the coal-tar pitch after middle temperature or pyrogenic distillation, and softening temperature is 40 ~ 90 DEG C, and carbon residue, at more than 25wt%, accounts for the 10wt% ~ 50wt% of asphalt stock total amount; The de-oiled asphalt that asphalt stock B is vacuum residuum, straight-run pitch, solvent de-asphalting process obtain, the mixture of one or more be in harmonious proportion in pitch, 25 DEG C of penetration degrees of asphalt stock B are 20 ~ 2001/10mm, softening temperature is 30 ~ 75 DEG C, accounts for the 50wt% ~ 90wt% of material asphalt total amount.
2. according to Asphalt composition particle according to claim 1, it is characterized in that: Asphalt composition particle median size≤100mm.
3. according to Asphalt composition particle according to claim 1, it is characterized in that: described treated starch is one or more in phosphate ester starch, carboxymethyl starch or cationic starch.
4. according to Asphalt composition particle according to claim 1, it is characterized in that: described water soluble fibre is one or more in carboxymethyl cellulose, polyvinyl alcohol fiber.
5. according to Asphalt composition particle according to claim 1, it is characterized in that: described promotor is one or more in modification bay alcohol radical sodium sulfate, secondary alcohol groups sodium sulfate, mixed fatty alcohol sodium sulfate, Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, sodium lignosulfonate or calcium lignin sulphonate.
6. according to Asphalt composition particle according to claim 1, it is characterized in that: described oxygen-containing gas is air, oxygen rich gas or oxygen.
7. according to Asphalt composition particle according to claim 1, it is characterized in that: asphalt stock A mixes in premixing tank with oxygen-containing gas, premixing tank is the encloses container of outlet with throttling valve.
8. according to Asphalt composition particle according to claim 1, it is characterized in that: the mixing temperature of asphalt stock A and oxygen-containing gas is 80 ~ 180 DEG C, and blend pressure is 0.1 ~ 0.5MPa, and mixing time is 1 ~ 60 minute.
9. according to Asphalt composition particle according to claim 7, it is characterized in that: the mode that the asphalt stock A of mixing oxygen-containing gas enters oxidation reactor is spray regime.
10. according to Asphalt composition particle according to claim 9, it is characterized in that: described course of injection is the throttling valve by opening premixing tank exit, the raw material A being rich in gas is ejected in oxidation reactor.
11., according to Asphalt composition particle according to claim 1, is characterized in that: described oxidation reactor is batch oxidation still or continous way oxidizing tower.
12., according to Asphalt composition particle according to claim 1, is characterized in that: oxidation reaction condition is: gas flow is 0.05 ~ 0.5m
3 .kg
-1 .h
-1, oxidizing temperature is 200 ~ 320 DEG C, and oxidization time is 3 ~ 10 hours.
The preparation method of 13. 1 kinds of Asphalt composition particle according to claim 1, is characterized in that comprising following content: high softening point bitumen, treated starch and/or water soluble fibre and promotor are carried out co-grinding, obtains Asphalt composition particle.
14., according to preparation method according to claim 13, is characterized in that: disintegrating apparatus is stirring-type or impact type mechanical crusher, and pulverizing temperature is normal temperature, grinding time 10 ~ 60 seconds.
15. 1 kinds of Asphalt composition particle according to claim 1 are applied in deep layer drilling fluid system.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524476B (en) * | 2014-10-22 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of modified asphalt composite particle and preparation method |
| CN105585864B (en) * | 2014-10-22 | 2017-10-03 | 中国石油化工股份有限公司大连石油化工研究院 | A kind of latex modified asphalt composition grain and preparation method thereof |
| CN105585862B (en) * | 2014-10-22 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of modified asphalt composite particle and preparation method thereof |
| CN105585857B (en) * | 2014-10-22 | 2017-10-03 | 中国石油化工股份有限公司 | A kind of preparation method of high softening point bitumen particle |
| CN105585858B (en) * | 2014-10-22 | 2017-10-03 | 中国石油化工股份有限公司 | A kind of modified asphalt composite particle and preparation method thereof |
| CN105585861B (en) * | 2014-10-22 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of modified pitch particle and preparation method thereof |
| CN115537032B (en) * | 2021-06-30 | 2023-06-16 | 中国石油化工股份有限公司 | SBS modified asphalt with excellent ageing resistance and preparation method thereof |
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