CN106479463A - Retarded crosslinking high intensity frozen glue profile-controlling and plugging agent - Google Patents
Retarded crosslinking high intensity frozen glue profile-controlling and plugging agent Download PDFInfo
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- CN106479463A CN106479463A CN201610831946.1A CN201610831946A CN106479463A CN 106479463 A CN106479463 A CN 106479463A CN 201610831946 A CN201610831946 A CN 201610831946A CN 106479463 A CN106479463 A CN 106479463A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
Abstract
The invention discloses a kind of retarded crosslinking high intensity frozen glue profile-controlling and plugging agent, its component and mass percent composition are as follows：Hydrophobic associated polymer 0.3%～0.6%, melmac crosslinking agent 0.3%～0.6%, Phenolic crosslinkers 0.03%～0.05%, oxygen scavenger 0.2%～0.4%, delayed crosslinker 0.1%～0.3%, dehydration inhibitor 0.1%～0.2% and excess water, the mass percent sum of each component is 100%, wherein, the Phenolic crosslinkers are one of resorcinol and hydroquinones or combine, oxygen scavenger is thiocarbamide and sodium sulfite and one of sodium hydrogensulfite or combine, delayed crosslinker is one of ammonium chloride and sodium trimetaphosphate or combines, dehydration inhibitor is one of sodium malonate or sodium salicylate or combination.The gelation time of frozen glue provided by the present invention is at 6 days and adjustable above, and after plastic, range estimation gel strength is at least up to H rank, and thermal stability is excellent, not dehydration after 60 DEG C～90 DEG C heat treatment 270 days, can meet the needs of most oil deposit deep part transfer drives.
Description
Technical field：
The present invention relates to a kind of hydrophobic associated polymer blocking agent, more particularly to a kind of retarded crosslinking high intensity frozen glue, belong to oil
Field technical field of chemistry.
Background technology：
In oilfield development process, after oil reservoir primary energy starts to reduce, need manually to supplement energy to stratum, i.e., to storage
Oil-bearing stratum flooding, to improve oil recovery factor.However, due to the anisotropism on stratum and the difference of oil and water mobility ratio or mining type
Improper, so that injection water is unevenly advanced along high permeability zone or high permeability zones, cause well water too early, until water logging.At present,
The most of waterflooding oil fields of China have been enter into high water cut stage.According to statistics, China's oil well production averagely aqueous reached 80% with
On, some old fileds of eastern region are aqueous to have reached more than 90%, and nearly the 90% of crude oil in China total amount originates from waterflooding extraction oil
Field.Therefore closure water breakthrough becomes the key for improving oil recovery factor.Profile control and water plugging controls the conventional measure of water as oil field, permissible
Raising formation pressure is played, the sweep efficiency of injection water is improved, so as to reach the effect for improving oil recovery factor.Polymer gel
Blocking agent becomes the most widely used water shutoff agent at present because which is cheap, preparation simple, construction effect is good.At present, China
The most frequently used polymer gel has phenolic aldehyde frozen glue, inorganic chromium gel and organic chrome jelly.However, although phenolic aldehyde frozen glue plastic is strong
Degree is high, in view of phenol, aldehydes toxicity and excitant are larger, onsite application is less, can be replaced by hydroquinones, resorcinol at present
Substituting phenol, methenamine substitute formaldehyde as crosslinking agent, but polyhydroxy phenol price is high, considerably increases production cost.Inorganic
Chromium gel system can be by controlling redox reaction by Cr6+Produce Cr3+Extend gelation time, but gelling strength is relatively
Weak, long-term thermal stability is poor, and is not suitable for high salinity reservoirs.It is relative that Organic Chromium can form gelation time as crosslinking agent
Longer frozen glue, but normally only it is applied to system of the temperature less than 60 DEG C, its cost intensive, prepare complicated, poor operability.Cause
This develop a kind of new retarded crosslinking high intensity gel plugging agent for solve China's deep oil well go out water problems have important
Meaning.
Content of the invention：
For the deficiencies in the prior art, it is an object of the invention to provide a kind of retarded crosslinking high intensity frozen glue profile-controlling and plugging agent.
The purpose of the present invention is realized by following technical scheme：
The retarded crosslinking high intensity frozen glue profile-controlling and plugging agent, by hydrophobic associated polymer, melmac crosslinking agent, phenol
Class crosslinking agent, oxygen scavenger, delayed crosslinker, dehydration inhibitor and water composition, the mass percent composition of each component are as follows:
Hydrophobic associated polymer 0.3%～0.6%；
Melmac crosslinking agent 0.3%～0.6%；
Phenolic crosslinkers 0.03%～0.05% are resorcinol and one of hydroquinones or combine；
Oxygen scavenger 0.2%～0.4% is thiocarbamide and one of sodium sulfite or combine；
Delayed crosslinker 0.1%～0.3% is ammonium chloride and one of sodium trimetaphosphate or combine；
Dehydration inhibitor 0.1%～0.2% is sodium malonate and one of sodium salicylate or combine；
Water, surplus；
The mass percent sum of each component is 100%.
The relative molecular mass of the preferred hydrophobic associated polymer of the present invention is 800 × 104～1200 × 104.
The preparation method of above-mentioned retarded crosslinking high intensity frozen glue is as follows：
1st, hydrophobic associated polymer is fully dissolved in running water by proportioning in beaker under room temperature, seals standby；Again
By proportioning by melmac crosslinking agent, Phenolic crosslinkers, oxygen scavenger, delayed crosslinker, dehydration inhibitor and excess water
Mixing and stirring, seals standby.
2nd, above two solution mixing and stirring is obtained plastic liquid.
3rd, by above-mentioned become glue be placed in ampoule bottle, with alcohol blast burner sintering sealing, be placed in 60 DEG C～90 DEG C of baking oven
Aging 6 days and obtain final product retarded crosslinking high intensity frozen glue profile-controlling and plugging agent of the present invention above.
The invention has the beneficial effects as follows：
1st, melmac crosslinking agent used in the present invention contains triazine ring structure, due to conjugation so that each C-
N bond distance tends to homogenization, and the π bonding orbital of heteroaromatic has stronger interaction with two neighbouring π bonding orbitals, this
Interact and substantially increase the stability of cross-linking system.It is liquid under resin cross-linking agent normal temperature, with instant in water
Property, compared with conventional phenolic crosslinkers, significantly reduces difficulty of construction.
2nd, hydrophobic associated polymer always contains hydrophobic grouping, and this amphiphilic structure of polymer causes polymer macromolecule chain
The supermolecule dynamic physical cross-linked network structure based on the intra/inter- association of molecule is formed, shows preferable endurance of cutting
Energy.Due to containing hydrophobic grouping, become gelatin viscosity low, injection efficiency is good, can meet the needs of deep profile controlling.
3rd, carry out of acid adding catalysed promoted cross-linking reaction be typically chosen during plastic under the conditions of relatively low reservoir temperature, but simultaneously
There is certain defect.On the one hand, after acid adding, gelation time is wayward, and it is short to there is gelation time, easily dehydration or gelling strength
Low problem, this be due to excessive H+Presence destroy the stability of amide group cross-linked structure；On the other hand, acid cross-linked
Agent solution often corrodes ground corollary equipment and injection pipeline etc., which greatly increases development cost, while can be to reservoir
Cause certain injury.The present invention is using new catalyst resorcinol or/and hydroquinones, it is to avoid going out for the problems referred to above
Existing, resorcinol can participate in the carrying out of cross-linking reaction with hydroquinones so that cross-linking system have slowly be crosslinked, high intensity
Feature.
4th, gelation time of the present invention is at 6 days and adjustable (retarded crosslinking) above, and range estimation gel strength at least can reach H rank,
While not dehydration after being heat-treated 270 days under the conditions of 60 DEG C～90 DEG C in the water of salinity (60000mg/L) stratum, therefore, it is possible to
Meet the needs of most of oil deposit deep part transfer drive.
Specific embodiment：
In order to be more clearly understood from the present invention, now specific embodiments of the present invention are explained in detail, but this
Invention institute protection domain is not limited only to this.
Embodiment 1：
0.3g melmac, 0.03g resorcinol, 0.2g thiocarbamide, 0.1g ammonium chloride, 0.1g third is added in beaker
Diacid sodium, plus running water is to 50g, stirs so as to fully dissolve, then the mass concentration that 50g running water is prepared is
0.6% hydrophobic association polymer solution is mixed with above-mentioned solution, is uniformly mixing to obtain into glue, is taken 20ml and is loaded ampoule bottle
In, sintering sealing, it is placed in aging 6 days in 60 DEG C of baking oven, that is, obtains frozen glue of the present invention.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 1# and 2#, after water drive to pressure stability
Obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core pore-body
Product), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 60 DEG C of baking ovens aging 30 days and 180 days respectively, most
Water drive is distinguished afterwards to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%, meter
Reservoir core plugging rate E is calculated, experimental result is as shown in table 1：
1 embodiment of table, 1 shut-off capacity is tested
Embodiment 2：
0.4g melmac, 0.04g resorcinol, 0.3g thiocarbamide, 0.15g ammonium chloride, 0.15g is added in beaker
Sodium malonate, plus the 1%NaCl aqueous solution stirred to 50g so as to fully dissolve, then by 50g 1%NaCl solution
Mass concentration be that 0.6% hydrophobic associated polymer is mixed with above-mentioned solution, be uniformly mixing to obtain into glue, take 20ml loading
In ampoule bottle, sintering sealing, it is placed in aging 7 days in 65 DEG C of baking oven, obtains final product frozen glue of the present invention.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 3# and 4#, after water drive to pressure stability
Obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core pore-body
Product), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 65 DEG C of baking ovens aging 30 days and 180 days respectively, most
Water drive is distinguished afterwards to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%, meter
Reservoir core plugging rate E is calculated, experimental result is as shown in table 2：
2 embodiment of table, 2 shut-off capacity is tested
Embodiment 3：
0.5g melmac, 0.05g resorcinol, 0.3g thiocarbamide, 0.2g ammonium chloride, 0.2g third is added in beaker
Diacid sodium, plus the 3%NaCl aqueous solution stirred to 50g so as to fully dissolve, then by 50g 3%NaCl solution
Mass concentration is that 0.8% hydrophobic associated polymer is mixed with above-mentioned solution, is uniformly mixing to obtain into glue, takes 20ml and loads peace
In small jar bottle, sintering sealing, it is placed in aging 7 days in 70 DEG C of baking oven, that is, obtains frozen glue of the present invention.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 5# and 6#, after water drive to pressure stability
Obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core pore-body
Product), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 70 DEG C of baking ovens aging 30 days and 180 days respectively, most
Water drive is distinguished afterwards to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%, meter
Reservoir core plugging rate E is calculated, experimental result is as shown in table 3：
3 embodiment of table, 3 shut-off capacity is tested
Embodiment 4：
In beaker add 0.5g melmac, 0.05g resorcinol, 0.02g hydroquinones, 0.3g thiocarbamide,
0.2g ammonium chloride, 0.2g sodium malonate, 0.1g sodium salicylate, plus the 5%NaCl aqueous solution stirred to 50g so as to fully molten
Solution, then 50g is mixed with above-mentioned solution with the hydrophobic associated polymer that the mass concentration of 5%NaCl solution is 0.8%,
Glue is uniformly mixing to obtain into, is taken 20ml and loads in ampoule bottle, sintering sealing, it is placed in aging 8 days in 70 DEG C of baking oven, that is, obtains
Frozen glue of the present invention.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 7# and 8#, after water drive to pressure stability
Obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core pore-body
Product), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 70 DEG C of baking ovens aging 30 days and 180 days respectively, most
Water drive is distinguished afterwards to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%, meter
Reservoir core plugging rate E is calculated, experimental result is as shown in table 4：
4 embodiment of table, 4 shut-off capacity is tested
Embodiment 5：
In beaker add 0.6g melmac, 0.05g resorcinol, 0.02g hydroquinones, 0.3g thiocarbamide,
0.2g ammonium chloride, 0.1g sodium trimetaphosphate, 0.2g sodium malonate, 0.1g sodium salicylate, plus 5%NaCl+0.1%CaCl2Water-soluble
Liquid is stirred to 50g so as to fully dissolved, then by 50g 5%NaCl+0.1%CaCl2The mass concentration of solution
Hydrophobic associated polymer for 1.0% is mixed with above-mentioned solution, is uniformly mixing to obtain into glue, is taken 20ml and is loaded in ampoule bottle,
Sintering sealing, is placed in aging 8 days in 80 DEG C of baking oven, that is, obtains frozen glue of the present invention.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 9# and 10#, water drive is to pressure stability
After obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core hole
Volume), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 80 DEG C of baking ovens aging 30 days and 180 days respectively,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 5：
5 embodiment of table, 5 shut-off capacity is tested
Embodiment 6：
In beaker add 0.6g melmac, 0.05g resorcinol, 0.03g hydroquinones, 0.3g thiocarbamide,
0.2g sodium sulfite, 0.2g ammonium chloride, 0.1g sodium trimetaphosphate, 0.2g sodium malonate, 0.15g sodium salicylate, plus 5%NaCl+
0.1%CaCl2+ 0.1%MgCl2The aqueous solution is stirred to 50g so as to fully dissolved, then by 50g 5%NaCl+0.1%
CaCl2+ 0.1%MgCl2The mass concentration of solution is 1.2% hydrophobic associated polymer and above-mentioned solution mix and blend
Glue is uniformly obtained into, is taken 20ml and loads in ampoule bottle, sintering sealing, it is placed in aging 10 days in 90 DEG C of baking oven, that is, obtains this
Invent the frozen glue.
Shut-off capacity is investigated：
Investigate the shut-off capacity of frozen glue provided by the present invention.Specific experiment process is as follows：By internal diameter be 2.5cm, length
For 20cm two fill out sand tube filling quartz sand grains be obtained high and low ooze simulation core, be denoted as 11# and 12#, water drive is to pressure stability
After obtain original permeability k1, then by above-mentioned become glue inverse injection fill out sand tube in, injected slurry volume be 0.5PV (rock core hole
Volume), it is then injected into 0.3PV water and is replaced, afterwards fill out sand tube is placed in 90 DEG C of baking ovens aging 30 days and 180 days respectively,
Water drive is finally distinguished to pressure stability, measure stifled rear permeability k of simulation core2, and press formula E=(k1-k2)/k1* 100%,
Reservoir core plugging rate E is calculated, experimental result is as shown in table 6：
6 embodiment of table, 6 shut-off capacity is tested
Table 1 to table 6 test result indicate that：The frozen glue that the present invention is provided has excellent sealing characteristics under the high temperature conditions,
, more than 99%, sealing ratiod is more than 96% within 180 days for 30 days sealing ratiods of low permeability cores；30 days sealing ratiods of hypertonic rock core 97% with
On, sealing ratiod is more than 95% within 180 days.So the stratum to high low-permeability is respectively provided with good plugging effect, be conducive to original
The raising of oil recovery.
Claims (1)
1. a kind of retarded crosslinking high intensity frozen glue profile-controlling and plugging agent, it is characterised in that each component and its mass percent composition as follows：
Hydrophobic associated polymer 0.3%～0.6%, melmac crosslinking agent 0.3%～0.6%, Phenolic crosslinkers 0.03%～
0.05%th, oxygen scavenger 0.2%～0.4%, delayed crosslinker 0.1%～0.3%, dehydration inhibitor 0.1%～0.2% and surplus
Water, the mass percent sum of each component is 100%, and wherein, Phenolic crosslinkers are one of resorcinol and hydroquinones or group
Close, oxygen scavenger is thiocarbamide or one of sodium sulfite or sodium hydrogensulfite or combination, and delayed crosslinker is ammonium chloride and three metaphosphoric acids
One of sodium or combination, dehydration inhibitor are one of sodium malonate or sodium salicylate or combination, and preferred hydrophobic associated polymer
Relative molecular mass is 800 × 104～1200 × 104.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365573A (en) * | 2017-06-13 | 2017-11-21 | 中国石油天然气集团公司 | A kind of preparation method and application of middle low-temperature environment-friendly crosslinking agent |
| CN107502326A (en) * | 2017-09-04 | 2017-12-22 | 中国石油化工股份有限公司 | A kind of secondary cross-linking carries liquid |
| CN108300440A (en) * | 2018-02-09 | 2018-07-20 | 中国石油大学(华东) | Ontology jelly system that frozen glue dispersion nano-graphite breast is strengthened and combinations thereof and preparation method and application |
| CN109679602A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of frozen glue profile-controlling and plugging agent and preparation method thereof |
| CN109679604A (en) * | 2019-01-28 | 2019-04-26 | 中国石油大学(华东) | A kind of salt tolerant high-temperature resistant water gel and the preparation method and application thereof |
| CN109765143A (en) * | 2019-03-01 | 2019-05-17 | 延安中杰高新工贸有限公司 | A kind of evaluation method and device being classified profile control and water plugging effect |
| CN111286311A (en) * | 2020-03-03 | 2020-06-16 | 中国石油天然气股份有限公司 | Multiple cross-linking type polymer gel profile control agent and application thereof |
| CN113249102A (en) * | 2021-04-09 | 2021-08-13 | 中国石油大学(华东) | Slow cross-linking gel for profile control of medium-high temperature oil reservoir and preparation method thereof |
| CN114516737A (en) * | 2022-03-25 | 2022-05-20 | 西南石油大学 | Water-invasion-resistant cement slurry for cementing water-bearing stratum and preparation method thereof |
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| CN107365573A (en) * | 2017-06-13 | 2017-11-21 | 中国石油天然气集团公司 | A kind of preparation method and application of middle low-temperature environment-friendly crosslinking agent |
| CN107365573B (en) * | 2017-06-13 | 2020-03-31 | 中国石油天然气集团公司 | Preparation method and application of medium-low temperature environment-friendly cross-linking agent |
| CN107502326A (en) * | 2017-09-04 | 2017-12-22 | 中国石油化工股份有限公司 | A kind of secondary cross-linking carries liquid |
| CN109679602A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | A kind of frozen glue profile-controlling and plugging agent and preparation method thereof |
| CN108300440A (en) * | 2018-02-09 | 2018-07-20 | 中国石油大学(华东) | Ontology jelly system that frozen glue dispersion nano-graphite breast is strengthened and combinations thereof and preparation method and application |
| CN108300440B (en) * | 2018-02-09 | 2018-12-25 | 中国石油大学(华东) | Ontology jelly system that frozen glue dispersion nano-graphite cream is strengthened and combinations thereof and preparation method and application |
| US10414969B2 (en) | 2018-02-09 | 2019-09-17 | China University Of Petroleum (East China) | Colloidal nano-graphite-strengthened bulk gel system for dispersed particle gel and composition thereof |
| CN109679604B (en) * | 2019-01-28 | 2021-01-05 | 中国石油大学(华东) | Salt-resistant and high-temperature-resistant hydrogel and preparation method and application thereof |
| CN109679604A (en) * | 2019-01-28 | 2019-04-26 | 中国石油大学(华东) | A kind of salt tolerant high-temperature resistant water gel and the preparation method and application thereof |
| CN109765143A (en) * | 2019-03-01 | 2019-05-17 | 延安中杰高新工贸有限公司 | A kind of evaluation method and device being classified profile control and water plugging effect |
| CN111286311A (en) * | 2020-03-03 | 2020-06-16 | 中国石油天然气股份有限公司 | Multiple cross-linking type polymer gel profile control agent and application thereof |
| CN113249102A (en) * | 2021-04-09 | 2021-08-13 | 中国石油大学(华东) | Slow cross-linking gel for profile control of medium-high temperature oil reservoir and preparation method thereof |
| CN113249102B (en) * | 2021-04-09 | 2022-12-27 | 中国石油大学(华东) | Slow cross-linking gel for profile control of medium-high temperature oil reservoir and preparation method thereof |
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Application publication date: 20170308 |