CN102807849B - Gel plugging agent for deep profile control of higher temperature oil reservoir and preparation method of gel plugging agent - Google Patents
Gel plugging agent for deep profile control of higher temperature oil reservoir and preparation method of gel plugging agent Download PDFInfo
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Abstract
The invention relates to a gel plugging agent for deep profile control of a higher temperature oil reservoir, and a preparation method of the gel plugging agent. The gel plugging agent comprises 0.3-0.8 percent of nonionic polyacrylamide, 0.6-1.3 percent of a cross-linking agent A, 0.45-1.44 percent of a cross-linking agent B, 0.02-0.04 percent of a temperature stabilizer and 0.01-0.08 percent of a pH value regulator, wherein the cross-linking agent A is methenamine; the cross-ling agent B is hydroquinone or resorcinol; the temperature stabilizer is sodium thiosulfate, sodium bisulfite or sodium sulfite; and the pH regulator is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate. The gel plugging agent disclosed by the invention has strong temperature resisting performance and can be used for the profile control operation of the high temperature oil reservoir with 100-160DEG C; the gel plugging agent has the characteristics of high strength after being gelatinized, stronger plugging capability for the stratum and favorable thermal stability; and in addition, after the gel plugging agent is stood at the temperature of 130 DEG C for 90 days, the strength change is little and gel breaking and hydration are avoided.
Description
Technical field
The present invention relates to the agent of a kind of high-temperature oil reservoir water plugging and profile controlling, in particular for gel plugging agent of high-temperature oil reservoir deep water plugging and profile controlling and preparation method thereof.
Technical background
Along with the exploitation gradually in oil field, well water is day by day serious, and oil well is average moisture at present reaches more than 80%, so the work of profile control and water plugging obtains applying more and more widely.Be oilwell water shutoff or Profile Control in Injection Well at present the most effective means be all to utilize chemical agent, by chemical means, to water-yielding stratum is disconnected, carry out shutoff.Because oil recovery condition is more and more harsher, the water plugging profile control agent under development hot conditions has become the problem that must face.
Ploymer Gel Plugging Agent is simple because of its wide material sources, preparation, has become the organic water plugging profile control agent of the most widely used class of domestic and international research, and the polymkeric substance adopting is mainly polyacrylamide.Yet due to polyacrylamide meeting thermal destruction under hot environment, cause the cross-link intensity of frozen glue to reduce, effect of field application is affected.The frozen glue that the polyacrylamide polymer of take is in recent years host development mainly contains chromium gel, Zirconium gel, resol frozen glue, polymine frozen glue etc., the weak point of these frozen glue is after temperature surpasses 110 ℃, high temperature can destroy the network structure of polymer gel, cause the low and poor stability of the gel strength that forms, even cannot gelation.CN86108877A discloses a kind of Zirconium gel water sealing agent, gelatinizing agent polyacrylamide (PAM) or type methylene polyacrylamide (MPAM), consists of with cross-linking of inorganic zirconium compound.Injection technology adopts two-fluid process, simple process, and construction safety, and can block up and can separate.This blocking agent both can be used for oil well, carried out selective water shut-off; Can be used for again water injection well, adjust intake profile.Its Heat stability is good, water plugging rate is high, and adsorptivity is strong, water-fast washing away, validity period is long, and blocking agent nontoxicity and pungency are with low cost.
In inorganic blocking agent because silicate gel class configuration is convenient, the cheap water plugging and profile controlling operation that is widely used in oil field.Silicate be take water glass as main, utilizes water glass to react with activator or reacts generation silicic acid gel or precipitation with the calcium ions and magnesium ions in local water, plays the effect of the high seepage channel of shutoff.The silicate of take is that the advantage of main inorganic blocking agent is high temperature resistant, but that shortcoming is intensity is lower, and at high temperature gelation time is short, and blocking radius is little, is not suitable for carrying out deep profile controlling water blockoff.
CN102040979A discloses a kind of composite gel plugging agent, calcium lignin sulphonate, potassium bichromate, sodium-chlor, rice he, Repone K, water, consists of.It is stifled over the tune of 90 ℃ of oil reservoirs that this compound frozen glue gel plugging agent is not suitable for temperature.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of gel plugging agent that is applicable to high-temperature oil reservoir (100～160 ℃) deep water plugging and profile controlling and preparation method thereof.
Terminological interpretation:
Urotropine, chemistry vulkacit H by name.
Non-ionic polyacrylamide, refers to the polyacrylamide that degree of hydrolysis is less than 5%, notes by abridging as NPAM.
Technical scheme of the present invention is as follows:
, mass percent is composed as follows:
Non-ionic polyacrylamide 0.3～0.8%, linking agent A 0.6～1.3%, crosslinking agent B 0.45～1.44%, temperature stabilising agent 0.02%～0.04%, pH value conditioning agent 0.01%～0.08%, and the water of surplus;
Described linking agent A is urotropine, and crosslinking agent B is Resorcinol or Resorcinol;
Described temperature stabilising agent is Sulfothiorine, sodium bisulfite or S-WAT;
Described pH adjusting agent is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
Preferred according to the present invention, a kind of gel plugging agent, mass percent is composed as follows:
Non-ionic polyacrylamide 0.4～0.6%, linking agent A 0.6～1.2%, crosslinking agent B 0.48～1.2%, temperature stabilising agent 0.02%～0.04%, pH value conditioning agent 0.01%～0.08%, and the water of surplus;
Preferred according to the present invention, the relative molecular mass of described non-ionic polyacrylamide is 800 * 10
4～1200 * 10
4, degree of hydrolysis is 2%～4%.
Further preferred according to the present invention, crosslinking agent B is Resorcinol, temperature stabilising agent S-WAT, and pH value conditioning agent is sodium hydroxide.
The preparation method of gel plugging agent of the present invention, step is as follows:
(1) by proportioning, non-ionic polyacrylamide is added to the water and is stirred to dissolving completely, then add linking agent A, crosslinking agent B and temperature stabilising agent, stir; Must become glue;
(2) to adding concentration in the one-tenth glue of step (1), be pH adjusting agent solution adjust pH to 8.0～9.0 of 10wt%, obtain frozen glue and become glue.
Frozen glue of the present invention becomes glue, and at 110 ℃, gelation time is 20～36h, and gelation time is 7～23h at 130 ℃.
When frozen glue becomes glue pH value 8.0～8.5, be suitable for position, deep 30～40m and carry out shutoff, gelation time is 22～36h at 110 ℃, gelation time is 8～23h at 130 ℃.When frozen glue becomes glue pH value 8.5～9.0, be suitable for position, deep 20～30m and carry out shutoff, gelation time is 20～33h at 110 ℃, gelation time is 7～21h at 130 ℃.
Gel plugging agent of the present invention is applicable to high-temperature oil reservoir deep profile controlling water blockoff.
Technical characterstic of the present invention:
Gel plugging agent of the present invention adopts multiple crosslinking agent, the formaldehyde producing after Resorcinol or Resorcinol and urotropine hydrolysis reacts and generates resol intermediate, then form the frozen glue with tridimensional network with non-ionic polyacrylamide generation crosslinking reaction, 0.02%～0.04% temperature stabilising agent is for improving the temperature resistant capability of frozen glue, and be 0.01%～0.08% by regulating the massfraction of pH adjusting agent in becoming glue, for controlling the plastic effect of frozen glue.Gel plugging agent of the present invention is along with plastic liquid system pH value increases, and gelation time slightly shortens.
The present invention, by controlling the gelation time of blocking agent plastic system, makes it on stratum, carry out indepth plugging in position, different deep, and this blocking agent both can be used for oil well, carried out selective water shut-off; Can be used for again water injection well, adjust intake profile, thereby effectively improve formation heterogeneity, expand the swept volume of follow-up fluid, improve the recovery ratio of crude oil.The invention has the beneficial effects as follows:
Gel plugging agent of the present invention is compared with current similar frozen glue, and heat resistance is remarkable, can be used for the deep profile controlling water blockoff (being greater than the stratum of 20m apart from well distance) of 100 ℃～160 ℃ of high-temperature oil reservoir.And this gel plugging agent is not only prepared simply, gelation time and intensity can regulate according to field condition, and thermal stability is good, place 90 days Strength Changes at 130 ℃ little, without dehydration phenomenon.
Accompanying drawing explanation
Fig. 1 is the frozen glue photo that the product frozen glue of embodiment 5 becomes glue gelation time 22h at 110 ℃.
Fig. 2 is the frozen glue photo that the product frozen glue of embodiment 6 becomes glue gelation time 7.5h at 130 ℃.
Embodiment
Below in conjunction with embodiment, illustrate the present invention.But be not limited to this.
In embodiment, non-ionic polyacrylamide used (NPAM) relative molecular mass is 900 * 10
4～1000 * 10
4, degree of hydrolysis is 3%.
Embodiment 1:
At massfraction, be in 0.4% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.3g, then add Resorcinol pressed powder 0.3g, adding temperature stabilising agent S-WAT 0.015g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is that 10.0% sodium hydroxide solution (pH adjusting agent) 0.06g is adjusted to 8.01 by system pH, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 36h, and gelation time is 23h at 130 ℃.
Embodiment 2:
At massfraction, be in 0.5% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.4g, then add Resorcinol pressed powder 0.4g, adding temperature stabilising agent S-WAT 0.015g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is 10.0% sodium hydroxide solution (pH adjusting agent) 0.17g, system pH is adjusted to 8.48, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 25h, and gelation time is 11h at 130 ℃.
Embodiment 3:
At massfraction, be in 0.6% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.5g, then add Resorcinol pressed powder 0.5g, adding temperature stabilising agent S-WAT 0.015g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is that 10.0% sodium hydroxide solution (pH adjusting agent) 0.4g is adjusted to 8.92 by system pH, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 21h, and gelation time is 8h at 130 ℃.
Embodiment 4:
At massfraction, be in 0.5% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.4g, then add Resorcinol pressed powder 0.4g, adding temperature stabilising agent sodium bisulfite 0.010g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is 10.0% sodium hydroxide solution (pH adjusting agent) 0.15g, system pH is adjusted to 8.20, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 23h, and gelation time is 10h at 130 ℃.
Embodiment 5:
At massfraction, be in 0.6% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.5g, then add Resorcinol pressed powder 0.5g, adding temperature stabilising agent S-WAT 0.014g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is that 10.0% sodium hydroxide solution (pH adjusting agent) 0.4g is adjusted to 8.93 by system pH, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 22h, and gelation time is 9h at 130 ℃.
Embodiment 6:
At massfraction, be in 0.6% non-ionic polyacrylamide aqueous solution 50g, add while stirring urotropine pressed powder 0.6g, then add Resorcinol pressed powder 0.6g, adding temperature stabilising agent S-WAT 0.015g again and being stirred to medicine is all dissolved in the aqueous solution, finally adding massfraction is that 10.0% potassium hydroxide solution (pH adjusting agent) 0.46g is adjusted to 8.90 by system pH, and stirring and obtaining frozen glue of the present invention becomes glue.This frozen glue gelation time at 110 ℃ is 20h, and gelation time is 7.5h at 130 ℃.
Embodiment 7:
The shut-off capacity of gel plugging agent of the present invention, adopts fill out sand tube rock core to evaluate it, measures the sealing ratiod of different ingredients blocking agent.
Experimentation is: will long 20cm, three fill out sand tube of internal diameter 2.5cm are filled sand grains and are made simulation core, are designated as respectively B1, B2, B3, water drive to survey after pressure-stabilisation its stifled before rate of permeation k
w0, the frozen glue of then preparing different ingredients becomes glue, injects 0.3V
p(rock pore volume) becomes glue, injects subsequently 0.1V
pwater carried out replacement, finally fill out sand tube sealing was placed in 130 ℃ of electronic constant incubators, and after the complete plastic of blocking agent, water drive, to pressure-stabilisation, is surveyed the stifled rear rate of permeation k of rock core again
w1, and press formula
calculate reservoir core plugging rate E.Experimental result is in Table 1.
In blocking agent formula, linking agent A is urotropine, and crosslinking agent B is Resorcinol, and temperature stabilising agent is S-WAT, and pH adjusting agent is sodium hydroxide.
Table 1 blocking agent sealing ratiod experimental result
Experimental result shows, gel plugging agent of the present invention at high temperature has very strong sealing characteristics, can guarantee in site operation effectively shutoff most permeable zone, improves oil recovery factor.
Embodiment 8: the test of test in place well
Test pit basic condition, as table 2, is injected working fluid situation in Table 3, and construction effect is in Table 4.
Table 2 test pit basic condition
| Situation | Test pit |
| Commissioning date | On December 4th, 2008 |
| Oil Reservoir Types | Petroclastic rock |
| Completion mode | Well-cased perforating completion |
| Completion interval of well section (m) | 4776-4860，4880-5038 |
| Thickness situation | 15m |
| Formation temperature (℃) | 110 |
Table 3 test pit working fluid injects situation
Note: tensio-active agent is OP 10, and linking agent A is urotropine, and crosslinking agent B is Resorcinol, and temperature stabilising agent is S-WAT, and pH adjusting agent is sodium hydroxide, surplus be water.
The construction effect table of table 4 test pit
| Project | Test pit |
| Before stifled average day moisture (%) | 87 |
| Average day produce oil (t) before stifled | 3.5 |
| After stifled minimum day moisture (%) | 52.3 |
| The highest day produce oil (t) after stifled | 23 |
| Average daily precipitation (%) after stifled | 16 |
| Oil (t) on average increases day by day after stifled | 11.7 |
| Validity period (d) | 53 |
| Accumulative total oil increment (t) | 530 |
Site test results shows, the average oil offtake 11.7t that increases day by day after test pit is stifled, and average moisture content day falls 16%, so far, and validity period 53 days, accumulative total increases oily 530t, successful.
Claims (1)
1. the gel plugging agent for 100 ~ 160 ℃ of high-temperature oil reservoir deep water plugging and profile controllings, it is characterized in that mass percent is composed as follows: non-ionic polyacrylamide 0.4 ~ 0.6%, linking agent A 0.6 ~ 1.2%, crosslinking agent B 0.48 ~ 1.2%, temperature stabilising agent 0.02% ~ 0.04%, pH value conditioning agent 0.01% ~ 0.08%, and the water of surplus;
The relative molecular mass of described non-ionic polyacrylamide is 800 * 10
4~ 1200 * 10
4, degree of hydrolysis is 2% ~ 4%;
Described linking agent A is urotropine, and crosslinking agent B is Resorcinol or Resorcinol;
Described temperature stabilising agent is Sulfothiorine, sodium bisulfite or S-WAT;
Described pH adjusting agent is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate;
Described gel plugging agent is for being greater than the stratum of 20m apart from well distance;
When frozen glue becomes glue pH value 8.0 ~ 8.5, be suitable for position, deep 30～40m and carry out shutoff, gelation time is 22 ~ 36h at 110 ℃, gelation time is 8 ~ 23h at 130 ℃; When frozen glue becomes glue pH value 8.5 ~ 9.0, be suitable for position, deep 20～30m and carry out shutoff, gelation time is 20 ~ 33h at 110 ℃, gelation time is 7 ~ 21h at 130 ℃.
2. gel plugging agent as claimed in claim 1, is characterized in that non-ionic polyacrylamide relative molecular mass used is 900 * 10
4~ 1000 * 10
4, degree of hydrolysis is 3%.
3. gel plugging agent as claimed in claim 1, is characterized in that crosslinking agent B is Resorcinol, and temperature stabilising agent is S-WAT, and pH value conditioning agent is sodium hydroxide.
4. the preparation method of the gel plugging agent as described in claim 1～3 any one, step is as follows:
(1) by proportioning, non-ionic polyacrylamide is added to the water and is stirred to dissolving completely, then add linking agent A, crosslinking agent B and temperature stabilising agent, stir; Must become glue;
(2) to adding concentration in the one-tenth glue of step (1), be pH adjusting agent solution adjust pH to 8.0 ~ 9.0 of 10wt%, obtain.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104194754A (en) * | 2014-08-29 | 2014-12-10 | 荆州市大地石油科技有限责任公司 | Temperature-resistant salt-resistant HPAM/Cr<3+>/phenolic aldehyde compound crosslinked weak gel profile adjusting and water plugging agent and preparation method thereof |
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