CN106833573B - A kind of plugging agent and its preparation method and application - Google Patents

A kind of plugging agent and its preparation method and application Download PDF

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Publication number
CN106833573B
CN106833573B CN201611234660.1A CN201611234660A CN106833573B CN 106833573 B CN106833573 B CN 106833573B CN 201611234660 A CN201611234660 A CN 201611234660A CN 106833573 B CN106833573 B CN 106833573B
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plugging agent
oil
stirring
preparation
plugging
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CN106833573A (en
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刘强
张洪君
袁鹏
王浩
李�瑞
马昌明
郑猛
张俊
吕孝明
安岩
田野
赵剑飞
由春坤
冷冰
王磊
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China Petroleum and Natural Gas Co Ltd
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China Petroleum and Natural Gas Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/5045Compositions based on water or polar solvents containing inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5086Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

Abstract

The present invention provides a kind of plugging agent and its preparation method and application.By weight percentage, the raw material components of the plugging agent include the silicon mud of 8%-15%, the ageing oil of 5%-10%, the vermiculite power of 1%-3%, the walnut shell powder of 2%-4%, the sulfonated gilsonite powder of 1%-3%, the KYPAM polymer of 0.3%-0.8%, the anionic cellulose ether of 0.2%-0.6%, the alpha-olefin sodium sulfonate of 0.2%-0.5% and the water of surplus.Plugging agent provided by the invention and preparation method thereof can be realized the recycling of silicon mud and ageing oil resource, while the plugging agent prepared has the performances such as good heat-resistant salt-resistant, is capable of the technical application of entirely appropriate high temperature and high salt oil deposit oil-water well profile control and water plugging.

Description

A kind of plugging agent and its preparation method and application
Technical field
The invention belongs to oil-water well profile control and water plugging technology field, it is related to a kind of plugging agent and its preparation method and application.
Background technique
Silicon mud is product of the oil sludge after process, and oil sludge refers to the oil tank, settling tank, dirt of oil recovery factory's multi-purpose station Water pot, oil separator, landing bottom of pond mud, drilling well, operation, conduit wiring piercing and the ground sludge generated.Silicon mud has become oil field and opens One of the major pollutants generated during hair.In recent years, since the gradual perfection of Environmental Protection in China regulation and group company make The requirement of Green Development, silicon mud governing problem increasingly cause the concern of people.Liaohe Oil Field generates a large amount of oil sludges every year, due to Its is complex in composition, causes the separation of silicon mud difficult, and prior art processing cost is high, and harmless treatment is difficult, while Liaohe Oil Field is refined Oily factory's sump oil station ground crude oil, the oil slick on sewage precipitation tank top, the sump oil in Sewage Disposal recycling pond, dehydrator grease The a large amount of ageing oils of the generations such as interface intermediate layer, the complicated component of ageing oil, relative density, viscosity, asphalt colloid content Height also causes containing metals, these ingredients such as higher calcium, sodium, magnesium in addition in addition to containing a large amount of gum asphalt in ageing oil Ageing oil High water cut, dehydration are difficult.Therefore, there is an urgent need to develop a kind of processing techniques of high efficiency low cost, realize silicon mud and aging The recycling of oily resource.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of plugging agent and preparation method thereof and answer With.The preparation method of the plugging agent can be realized the recycling of silicon mud and ageing oil resource, while the plugging agent prepared is with good The performances such as good heat-resistant salt-resistant, are capable of the technical application of entirely appropriate high temperature and high salt oil deposit oil-water well profile control and water plugging.
The purpose of the present invention is achieved by the following technical programs:
The present invention provides a kind of plugging agent, and by weight percentage, the raw material components of the plugging agent include:
In above-mentioned plugging agent, it is preferable that the KYPAM polymer include KYPAM-1S, KYPAM-2S, KYPAM-3S and One of KYPAM-4S etc. or a variety of combinations are produced by Beijing perseverance dimerization work group company.
In above-mentioned plugging agent, it is preferable that the anionic cellulose ether may include carboxymethyl cellulose and/or poly- yin Ion fiber element, but not limited to this.
The present invention also provides the preparation methods of above-mentioned plugging agent comprising following steps:
Silicon mud and ageing oil are added in reaction kettle by step 1, and stirring at normal temperature is uniform;
Step 2 is added vermiculite power into reaction kettle and walnut shell powder, stirring at normal temperature is uniform;
Step 3 heats up reaction kettle, and sulfonated gilsonite powder, KYPAM polymer, anionic fibre are added into reaction kettle Plain ether and alpha-olefin sodium sulfonate are tieed up, is stirred evenly, is down to room temperature to temperature of reaction kettle, obtains plugging agent.
In above-mentioned preparation method, it is preferable that in step 1, the time of stirring is 10-20min;The revolving speed of stirring is 200-300rpm。
In above-mentioned preparation method, it is preferable that in step 2, the time of stirring is 5-10min;The revolving speed of stirring is 200- 300rpm。
In above-mentioned preparation method, it is preferable that in step 3, reaction kettle is warming up to 65-80 DEG C.
In above-mentioned preparation method, it is preferable that in step 3, the time of stirring is 10-15min;The revolving speed of stirring is 200-300rpm。
The present invention also provides application of the above-mentioned plugging agent in high temperature and high salt oil deposit oil-water well profile control and water plugging.
Silicon mud of the present invention is by-product of the oil sludge after process during oil extraction in oil field, from oil , there is good compatibility in hiding with oil reservoir, while siliceous mixture content is higher in silicon mud, effectively increases the plugging agent of preparation Heat resistance and plugging strength, while solving silicon mud processing problem, it realizes and recycles, it is stifled that silicon mud is used to prepare tune Profile control cost had both been saved in agent, is also saved silicon mud processing cost and is therefore had a good application prospect, all oil extraction in oil field Generated silicon mud may be applicable to the present invention in the process.
Ageing oil of the present invention be oil extraction in oil field during, after emulsification of crude oil, gradually coalesced at oil-water interfaces It is formed at certain thickness, generated ageing oil may be applicable to the present invention during all oil extraction in oil field.
Vermiculite power of the present invention is heated to be expanded, and volume increases 18-25 times, while curved in scratching, and have good Good expansion character and toughness, can be improved the plugging strength of plugging agent.
Lignin, cellulose and hemicellulose account for 95% or more in walnut shell powder of the present invention, and tune can be improved The mechanical strength of blocking agent increases plugging agent sealing characteristics.
Sulfonated gilsonite powder of the present invention is a kind of anionic high polymer, has good emulsifiability, temperature resistance Property is higher, simultaneously as sulfonated gilsonite powder contains sulfonic group, hydration is very strong, when being adsorbed on shale interface, can prevent The aquation dispersion of shale particle plays the role of that anti-collapse, not soluble in water part can fill pore throat again and plugging action is played in crack.
KYPAM polymer of the present invention thermal stability with higher and anti-salt property, degree of hydrolysis 20%- 30%, molecular weight is 12,000,000-1,600 ten thousand, its main feature is that being able to maintain higher for (>=90 DEG C) under the conditions of high-temperature oil reservoir Thermal stability.Under 90 DEG C of oxygen free conditions, viscosity retention ratio >=90% after 90 days compares conventional polymer under the conditions of high salinity Efficient Adhesive Promotion is more preferable, which saves 15-20%, greatly reduces operating cost, and can be effective Raising recovery ratio.
Anionic cellulose ether of the present invention has good heat-resistant stability and salt tolerance, while having good Good suspension, dispersibility, thickening property, gluing and emulsibility.
Alpha-olefin sodium sulfonate of the present invention has the characteristics of good biodegradability, nonhazardous, is a kind of Green product has preferable thermo-salt resistance, can control steamchanneling, overcome gravity segregation, reduce viscous fingering, Steam mobility is reduced, steam injection profile is adjusted, increases sweep efficiency, improves heavy oil recovery rate.
Plugging agent provided by the invention and preparation method thereof can be realized the recycling of silicon mud and ageing oil resource, make simultaneously Standby plugging agent has the performances such as good heat-resistant salt-resistant, is capable of the skill of entirely appropriate high temperature and high salt oil deposit oil-water well profile control and water plugging Art application.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
In raw material employed in embodiment, silicon mud and ageing oil are the by-product generated in the oil recovery process of Liaohe Oil Field; Other raw material components are commercially available.
Embodiment 1
The present embodiment provides a kind of plugging agents, and by weight percentage, the raw material components of the plugging agent include:
The present embodiment also provides the preparation method of above-mentioned plugging agent, carries out weighing raw material components according to aforementioned proportion, the system Preparation Method the following steps are included:
Silicon mud and ageing oil are added in reaction kettle by step 1, and stirring at normal temperature is uniform, mixing time 15min, stirring Revolving speed is 250rpm;
Vermiculite power and walnut shell powder are added into reaction kettle for step 2, and stirring at normal temperature is uniform, and mixing time 7min is stirred Mixing revolving speed is 250rpm;
Step 3 heats up reaction kettle, and sulfonated gilsonite powder, KYPAM-3S, polyanion fiber are added into reaction kettle Element and alpha-olefin sodium sulfonate, stir evenly, mixing time 13min, speed of agitator 250rpm is down to often to temperature of reaction kettle Temperature obtains plugging agent.
Following correlated performance evaluation is made to plugging agent manufactured in the present embodiment:
(1) thermal stability is tested
Plugging agent manufactured in the present embodiment is taken, behind its static 24 hours completely condensation, the survey of heat resistance is carried out to it Examination experiment, plugging agent test result under 200 DEG C of hot conditions are shown in Table 1.
Table 1
Ageing time (h) 24 36 48 60 90 142 360 480
Form Completely Completely Completely Completely Completely Completely Completely Aquation
Weight-loss ratio (%) 1.7 2.8 3.2 4.1 4.4 5.2 6.3 19.8
Shrinking percentage (%) 1.0 1.2 1.6 1.9 2.1 2.4 3.2 11.7
The test of above-mentioned heat resistance the result shows that: plugging agent provided in this embodiment in 200 DEG C of high temperature 15d, condensation Plugging agent form is almost unchanged, and after 20d, plugging agent structure changes, and starts high temperature aquation.It is therefore seen that the plugging agent With good high temperature resistance, the temperature condition of high-temperature oil reservoir can adapt to.
(2) salt resistant character evaluation experimental
According to the raw material components of the present embodiment, wherein water uses salinity for the water of 110000mg/L, is configured to adjust Blocking agent carries out salt resistant character test to it, tests viscosity change situation under the conditions of synthermal, and test result is shown in Table 2.
Table 2
Temperature, DEG C 90 110 130 150 170 190 200 220
Viscosity, mPas 38506 31214 25854 21203 15269 10158 8056 3685
By 2 experimental result of table it is found that plugging agent obtained is able to maintain larger viscosity, plays high intensity at 200 DEG C or less The effect of closure is more than after 200 DEG C in temperature, and viscosity decline is very fast, and blocking agent performance just starts to fail.Therefore the plugging agent is full Performance requirement under sufficient high temperature and high salt environment.
The present embodiment also provides application of the prepared plugging agent in high temperature and high salt oil deposit oil-water well profile control and water plugging.Specifically Are as follows: shutting out in Liaohe Oil Field, 813 pieces of 3 wells of field test are secondary, and scene is prepared using agitator tank, using pumping-in equipment injection well bottom, put down Within 1500 sides, injection pressure 12MPa, measure effective percentage adds up to increase 752 tons of oil, increases oil equal individual well dosage up to 90% or more Significant effect achieves good economic and social benefit, reduces environmental pollution, realizes the conjunction of silicon mud and ageing oil resource Reason effective use.
Embodiment 2
The present embodiment provides a kind of plugging agents, and by weight percentage, the raw material components of the plugging agent include:
The present embodiment also provides the preparation method of above-mentioned plugging agent, carries out weighing raw material components according to aforementioned proportion, the system Preparation Method the following steps are included:
Silicon mud and ageing oil are added in reaction kettle by step 1, and stirring at normal temperature is uniform, mixing time 12min, stirring Revolving speed is 200rpm;
Vermiculite power and walnut shell powder are added into reaction kettle for step 2, and stirring at normal temperature is uniform, and mixing time 6min is stirred Mixing revolving speed is 200rpm;
Step 3 heats up reaction kettle, and into reaction kettle be added sulfonated gilsonite powder, KYPAM-4S, carboxymethyl cellulose, Polyanion cellulose and alpha-olefin sodium sulfonate, stir evenly, mixing time 10min, speed of agitator 200rpm, wait react Kettle temperature degree is down to room temperature, obtains plugging agent.
Following correlated performance evaluation is made to plugging agent manufactured in the present embodiment:
(1) thermal stability is tested
Plugging agent manufactured in the present embodiment is taken, behind its static 24 hours completely condensation, the survey of heat resistance is carried out to it Examination experiment, plugging agent test result under 200 DEG C of hot conditions are shown in Table 3.
Table 3
Ageing time (h) 24 36 48 60 90 142 360 480
Form Completely Completely Completely Completely Completely Completely Completely Aquation
Weight-loss ratio (%) 1.5 2.6 3.1 4.1 4.3 5.4 6.2 20.5
Shrinking percentage (%) 1.1 1.3 1.5 1.8 2.0 2.3 3.1 12.6
The test of above-mentioned heat resistance the result shows that: plugging agent provided in this embodiment in 200 DEG C of high temperature 15d, condensation Plugging agent form is almost unchanged, and after 20d, plugging agent structure changes, and starts high temperature aquation.It is therefore seen that the plugging agent With good high temperature resistance, the temperature condition of high-temperature oil reservoir can adapt to.
(2) salt resistant character evaluation experimental
According to the raw material components of the present embodiment, wherein water uses salinity for the water of 120000mg/L, is configured to adjust Blocking agent carries out salt resistant character test to it, tests viscosity change situation under the conditions of synthermal, and test result is shown in Table 4.
Table 4
Temperature, DEG C 90 110 130 150 170 190 200 220
Viscosity, mPas 35957 30102 24236 18526 13287 9215 7248 3326
By 4 experimental result of table it is found that plugging agent obtained is able to maintain larger viscosity, plays high intensity at 200 DEG C or less The effect of closure is more than after 200 DEG C in temperature, and viscosity decline is very fast, and blocking agent performance just starts to fail.Therefore the plugging agent is full Performance requirement under sufficient high temperature and high salt environment.
The present embodiment also provides application of the prepared plugging agent in high temperature and high salt oil deposit oil-water well profile control and water plugging.Specifically Are as follows: in 2 well of Block Du 84, Liaohe Oilfield field test, scene is prepared using agitator tank, average using pumping-in equipment injection well bottom Within 1800 sides, injection pressure 13MPa, measure effective percentage adds up to increase 512 tons of oil individual well dosage up to 93% or more, increases oil effect Fruit is significant, achieves good economic and social benefit, reduces environmental pollution, realizes the reasonable of silicon mud and ageing oil resource Effective use.
In conclusion plugging agent provided by the invention and preparation method thereof can be realized the benefit again of silicon mud and ageing oil resource With, while the plugging agent prepared has the performances such as good heat-resistant salt-resistant, it being capable of entirely appropriate high temperature and high salt oil deposit oil-water well tune Cut open the technical application of water blockoff.

Claims (9)

1. a kind of plugging agent, by weight percentage, the raw material components of the plugging agent include:
2. plugging agent according to claim 1, it is characterised in that: the KYPAM polymer includes KYPAM-1S, KYPAM- One of 2S, KYPAM-3S and KYPAM-4S or a variety of combinations.
3. plugging agent according to claim 1, it is characterised in that: the anionic cellulose ether includes carboxymethyl cellulose Element and/or polyanion cellulose.
4. the preparation method of the described in any item plugging agents of claim 1-3 comprising following steps:
Silicon mud and ageing oil are added in reaction kettle by step 1, and stirring at normal temperature is uniform;
Step 2 is added vermiculite power into reaction kettle and walnut shell powder, stirring at normal temperature is uniform;
Step 3 heats up reaction kettle, and sulfonated gilsonite powder, KYPAM polymer, anionic cellulose are added into reaction kettle Ether and alpha-olefin sodium sulfonate, stir evenly, obtain plugging agent.
5. the preparation method according to claim 4, it is characterised in that: in step 1, the time of stirring is 10-20min; The revolving speed of stirring is 200-300rpm.
6. the preparation method according to claim 4, it is characterised in that: in step 2, the time of stirring is 5-10min; The revolving speed of stirring is 200-300rpm.
7. the preparation method according to claim 4, it is characterised in that: in step 3, reaction kettle is warming up to 65-80 DEG C.
8. the preparation method according to claim 4, it is characterised in that: in step 3, the time of stirring is 10-15min; The revolving speed of stirring is 200-300rpm.
9. application of any one of the claim 1-3 plugging agent in high temperature and high salt oil deposit oil-water well profile control and water plugging.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1927991A (en) * 2006-09-11 2007-03-14 大庆油田有限责任公司 Water plugging agent for water injection well preparing from discarded oil-containing sludge
CN101898860A (en) * 2010-08-05 2010-12-01 武汉工程大学 Inorganic profile control agent with oil sludge and application method thereof
CN103965848A (en) * 2014-04-29 2014-08-06 中国石油大学(华东) Composite profile control agent and preparation method thereof
CN104745162A (en) * 2015-02-26 2015-07-01 东北石油大学 Emulsified and cross-linked oil-containing sludge profile control agent
CN105038746A (en) * 2015-06-25 2015-11-11 西安石油大学 Preparation method of jelly-type oily sludge profile control agent
CN105112033A (en) * 2015-08-21 2015-12-02 中国石油天然气股份有限公司 Plugging control agent prepared by oil residues or oily sewage and preparation method thereof
CN105112035A (en) * 2015-08-21 2015-12-02 中国石油天然气股份有限公司 Selective water blocking agent prepared from oil residues or sludge containing oil and preparation method thereof
CN105368421A (en) * 2015-11-19 2016-03-02 里群 Non-resin type profile control agent and application thereof in petroleum exploitation process

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1927991A (en) * 2006-09-11 2007-03-14 大庆油田有限责任公司 Water plugging agent for water injection well preparing from discarded oil-containing sludge
CN101898860A (en) * 2010-08-05 2010-12-01 武汉工程大学 Inorganic profile control agent with oil sludge and application method thereof
CN103965848A (en) * 2014-04-29 2014-08-06 中国石油大学(华东) Composite profile control agent and preparation method thereof
CN104745162A (en) * 2015-02-26 2015-07-01 东北石油大学 Emulsified and cross-linked oil-containing sludge profile control agent
CN105038746A (en) * 2015-06-25 2015-11-11 西安石油大学 Preparation method of jelly-type oily sludge profile control agent
CN105112033A (en) * 2015-08-21 2015-12-02 中国石油天然气股份有限公司 Plugging control agent prepared by oil residues or oily sewage and preparation method thereof
CN105112035A (en) * 2015-08-21 2015-12-02 中国石油天然气股份有限公司 Selective water blocking agent prepared from oil residues or sludge containing oil and preparation method thereof
CN105368421A (en) * 2015-11-19 2016-03-02 里群 Non-resin type profile control agent and application thereof in petroleum exploitation process

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