CN110437818A - A kind of broken glue activator and preparation method thereof suitable for 20-50 DEG C of reservoir fracturing - Google Patents
A kind of broken glue activator and preparation method thereof suitable for 20-50 DEG C of reservoir fracturing Download PDFInfo
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- CN110437818A CN110437818A CN201910781885.6A CN201910781885A CN110437818A CN 110437818 A CN110437818 A CN 110437818A CN 201910781885 A CN201910781885 A CN 201910781885A CN 110437818 A CN110437818 A CN 110437818A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C233/00—Carboxylic acid amides
- C07C233/01—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
- C07C233/30—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by doubly-bound oxygen atoms
- C07C233/33—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by doubly-bound oxygen atoms with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by a carbon atom of a six-membered aromatic ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D257/00—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms
- C07D257/02—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms not condensed with other rings
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
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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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/26—Gel breakers other than bacteria or enzymes
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Abstract
The invention discloses a kind of broken glue activator suitable for 20-50 DEG C of reservoir fracturing, which is soluble Ag ionic complex.The complex compound that the ligand B of structure shown in ligand A or formula II of the activator for structure shown in silver nitrate and formula I is formed；The dosage mass ratio of silver nitrate and ligand A or ligand B are 3-5:20-35.The preparation method of activator is: ligand A or B being dissolved in the methanol aqueous solution of the 60-75% containing methanol quality, are heated to 50-70 DEG C, adjusting pH is 4-5, and AgNO is added3, stir evenly, adjusting pH with ammonium hydroxide is 7-8 to get to activator.The mass percent of ligand A or B in methanol aqueous solution is 20-35%.AgNO3Mass percent is 3-5% in methanol aqueous solution.The present invention is to provide a kind of low temperature to break glue activator, and the activator can activate gel breaker (NH in 20-50 DEG C of low temperature reservoir4)2S2O8Broken glue reaction.
Description
Technical field
The present invention relates to oil-gas mining technical field, especially a kind of broken glue activation suitable for 20-50 DEG C of reservoir fracturing
Agent and preparation method thereof.
Background technique
With the development of exploration and development technology, Low permeable oil and gas reservoirs of the permeability lower than 50mD are increasingly becoming petroleum reserves increasing
Long main body.The whole world is dispersed with a large amount of Low permeable oil and gas reservoirs, and stock number accounts for about the 20%-60% of basin resource, such as adds
The extension oil field in the oil field Pa Binna and China put on airs, Changqing oilfields etc..
The major alterations means of low permeability oil and gas field exploitation are hydraulic fracturing process, this technology has had accumulated more than 60 years warps
It tests, is widely used in oil field prospecting and exploitation.The specific embodiment of hydraulic fracturing process is: being injected and is carried by pit shaft
Then fracturing liquid rubber-breaking is returned row to strut and enter the oil storage stratum of cracking by the high pressure viscous fluid (fracturing fluid) of proppant
Ground is gone back to, and proppant is then trapped among stratum, accumulation forms excellent connection gap, produces permanence taking human as ground
The permeability of oil gas is improved in high water conservancy diversion rate crack, is finally reached the purpose of volume increase.
In the low-permeability oil deposit of China's discovery at present, low-temperature reservoir of the buried depth less than 1000m accounts for about 5.2%.For
Such hypotonic shallow oil reservoir of low temperature, the maximum difficult point that implement pressing crack construction is exactly that reservoir temperature is too low (go into the well by ordinary circumstance
Temperature is 30 DEG C -50 DEG C, and the well temperature of part well is even as low as 25 DEG C -30 DEG C).Reservoir temperature is lower, and fracturing liquid rubber-breaking rate is got over
Slowly, discharge speed is also smaller, and it is also lower to return scheduling degree, finally damages to reservoir.
In conventional pressing crack construction, usually make the gel breaker of fracturing fluid with ammonium persulfate.But under cryogenic,
(NH4)2S2O8Difficulty is decomposed, enough free radicals can not be generated.This directly affects fracturing liquid rubber-breaking effect, prevents it from abundant
Degradation, so that the original permeability of flow conductivity and stratum to proppant pack damages, leads to well capacity processed
Sharp fall.
Slow, the too long defect of gel breaking time in view of conventional guar gum fracturing fluid oxidation gel breaker glue rate broken at low temperature,
Domestic and international expert has developed a variety of new type low temperatures that can be applied to low temperature environment and breaks glue technology, to improve the effect of the broken glue under low temperature
Rate.Currently, there are mainly three types of new type low temperatures to break glue technology: low-temp activation breaks glue, enzyme breaks glue and capsule breaker.Wherein enzyme breaks glue
Agent Applicable temperature is between 20-90 degrees Celsius, and higher cost, and execute-in-place is complicated；Capsule breaker is changed under cryogenic
Reaction rate is lower, and dosage is larger, so that pressure break high expensive.Therefore it is broken in glue technology in these three low temperature, at present scene
Most widely used is that low-temp activation breaks colloid system.But the broken glue of low temperature currently in use in have been developed that now and production
Ammonium persulfate dosage and the dosage of low-temp activation agent needed for activation systems are all larger, and it improves fracturing liquid rubber-breaking rate, shorten
The ability of gel breaking time can't fully meet the requirement of site operation.Therefore we need to develop a kind of more efficient low temperature
Activation systems, making it not only can be reduced the dosage of ammonium persulfate, but also the fracturing fluid that can also improve low temperature well to a greater degree is broken
Glue rate shortens gel breaking time, to reduce damage of the breaking glue solution to oil field stratum.
Summary of the invention
It is an object of the invention to ammonium persulfate dosage and low-temp activations needed for breaking glue activation systems for existing low temperature
The dosage of agent is all larger, and it improves fracturing liquid rubber-breaking rate, and the ability for shortening gel breaking time can't fully meet scene and apply
The technological deficiency of the requirement of work provides a kind of broken glue activator of the low temperature suitable for 20-50 DEG C of reservoir fracturing.
It is a further object to provide a kind of above-mentioned low temperature suitable for 20-50 DEG C of reservoir fracturing to break glue activator
Preparation method.
Low temperature provided by the invention suitable for 20-50 DEG C of reservoir fracturing breaks the Ag ion that glue activator is a kind of solubility
Complex compound.The activator be structure shown in silver nitrate and formula I ligand A or formula II shown in structure ligand B formed in alkalinity
Under the conditions of be stabilized complex compound:
In formula, R is H or CH3。8,11-tetraazacylotetradeca-7,11-diene
Preferably, the dosage mass ratio of the silver nitrate and ligand A or ligand B are 3-5:20-35.
The molecular structural formula for the complex compound that silver nitrate and ligand A are formed is shown in formula III:
The molecular structural formula for the complex compound that silver nitrate and ligand B are formed is shown in formula IV:
In formula, R is H or CH3。
The preparation method of the above-mentioned broken glue activator suitable for 20-50 DEG C of reservoir fracturing, comprises the concrete steps that: by ligand A
Or B is dissolved in the methanol aqueous solution of the 60-75% containing methanol quality, is heated to 50-70 DEG C, is used lemon acid for adjusting pH for 4-5, is added
Enter AgNO3, stir evenly, adjusting pH with ammonium hydroxide is 7-8 to get to activator.
Preferably, mass percent of the ligand A or ligand B in methanol aqueous solution is 20-35%.AgNO3In
Mass percent is 3-5% in methanol aqueous solution.Preferably 60 DEG C of heating temperature.
Compared with prior art, the invention has the beneficial effects that:
It is Ag that low temperature of the invention, which breaks glue activator,+The complex compound formed with ligand, metal Ag+Outermost layer d energy level electronics energy
Amount is higher, is unpaired electron again in addition, and structural instability has stronger reproducibility.Ag+(NH can be reduced4)2S2O8Reaction
Activation energy, Ag+Activate S2O8 2-Generate free radicals SO4·-And OH, improve (NH4)2S2O8Reaction rate at low temperature, thus
So that broken glue reaction at low temperature can be gone on smoothly.Moreover, low-temp activation agent activates (NH4)2S2O8High price mistake generated afterwards
Cross metal cation Ag2+Also redox reaction can occur with organic matter free radical, so that reducing metal is cationic.
Ag+Although (NH can be accelerated4)2S2O8Decomposition at low temperature, but it can under alkaline environment with OH-React life
It is precipitated at AgOH, and the AgOH generated is extremely unstable, and decomposes and produce the silver oxide solid of brown.This is not only caused
AgNO3Waste, while silver oxide solid generated also causes pollution to fracturing fluid.Therefore, the present invention using ligand A or
Ligand B and Ag+Complex compound is formed as activator；The complex compound is water-soluble substances, can be also stabilized under alkaline condition,
It avoids and generates AgOH precipitating, expand the use scope that low temperature breaks glue activator.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
One, embodiment is prepared
Embodiment 1
A kind of preparation method of the broken glue activator suitable for 20-50 DEG C of reservoir fracturing, comprises the concrete steps that: ligand A is molten
(mass percent of the ligand A in methanol aqueous solution is 20%), heating in the methanol aqueous solution of the 60-75% containing methanol quality
It to 60 DEG C, uses lemon acid for adjusting pH for 4-5, AgNO is added3, AgNO3Mass percent is 3% in methanol aqueous solution, stirring
Uniformly, adjusting pH with ammonium hydroxide is 7-8 to get to the complex compound activator A being stabilized under alkaline condition.Ligand A structural formula
It is as follows:
Embodiment 2bis (benzaidehyde) (L)
A kind of preparation method of the broken glue activator suitable for 20-50 DEG C of reservoir fracturing, comprises the concrete steps that: ligand B is molten
In the methanol aqueous solution of the 60-75% containing methanol quality, mass percent of the ligand B in methanol aqueous solution is 35%, heating
It to 60 DEG C, uses lemon acid for adjusting pH for 4-5, AgNO is added3, AgNO3Mass percent is 5% in methanol aqueous solution, stirring
Uniformly, adjusting pH with ammonium hydroxide is 7-8 to get to the complex compound activator B being stabilized under alkaline condition.Ligand B structure formula
It is as follows:
Two, activator performance test 8,11-tetraazacylotetradeca-7,11-diene
The performance of activator A and activator B prepared by testing example 1 and 2.Experimental method mainly includes following two step
It is rapid:
(1) preparation of frozen glue
Base fluid: 0.4% hydroxypropyl guar gum+(0.02%-0.032%) NaOH (adjusting pH value to 11)+0.1%HCHO+
The low-temp activation agent (activator A or activator B) of 0.3% demulsification cleanup agent+1%KCl+ various concentration.
Crosslinking agent: 1% borax；
Gel breaker: 200ppm (NH4)2S2O8；
Crosslinking ratio: 100:5；
(2) measurement of static gel breaking time
Prepared frozen glue is packed into closed container, being put into thermostat temperature is respectively 20 DEG C, 40 DEG C and 50 DEG C
Heated at constant temperature in electric thermostat makes fracturing fluid break glue under thermostat temperature (apparent viscosity of breaking glue solution is less than 5mPa.s).Note
From glue is started brokenly to the time for breaking cementing beam under record, which is exactly the static gel breaking time of fracturing fluid.Test is at least heavy every time
It is multiple to carry out primary, it is subject to its gel breaking time that is averaged.Test result is shown in Tables 1 and 2.
Table 1, the static gel breaking time of the fracturing fluid containing various concentration activator A at different temperatures
Table 2, the static gel breaking time of the fracturing fluid containing various concentration activator B at different temperatures
By Tables 1 and 2 it is found that being far below un-activation added with the static gel breaking time of the low-temp activation system of activator A or B
Broken colloid system, this illustrates that activator of the invention can accelerate (NH4)2S2O8It decomposes, improves Gel Breakdown rate.For containing
The frozen glue of same concentrations activator, broken glue temperature is lower, then static gel breaking time is longer.At a temperature of same broken glue, frozen glue
Smaller then its static gel breaking time of the concentration of contained activator is longer.At 50 DEG C, 5ppm activator A just can be by the broken glue of frozen glue
Time foreshortens to 300min, and the gel breaking time of frozen glue just can be foreshortened to 296min by 5ppm activator B.20ppm activator A just can
The gel breaking time of frozen glue is foreshortened into 140min, the gel breaking time of frozen glue just can be foreshortened to 142min by 20ppm activator B, can
To reach demand of the conventional pressure break scale to gel breaking time.Furthermore experiment is it has also been found that containing only 10ppm activator and being free of (NH4)2S2O8Blank system can not break glue, this illustrates that activator itself cannot degrade frozen glue, cannot independently use.
Table 3 is containing various concentration AgNO3Fracturing fluid static gel breaking time at different temperatures.Experimental test procedures
Same Tables 1 and 2.As can be seen from Table 3, individual AgNO3To (NH4)2S2O8Just there is activation, improve Gel Breakdown speed
Rate.But work as AgNO3Concentration when being more than 10ppm, even if continuing growing AgNO3Concentration to 20ppm, AgNO3To (NH4)2S2O8Activation be not obviously improved but, AgNO3Concentration 10ppm and when 20ppm, the fracturing fluid break time differs very
It is small.This is because: as Ag in solution+When concentration is lower, AgOH generated is fewer, the silver oxide of brown made of decomposing
Solid is also less, all Ag+Activation can be played.But work as Ag+Concentration when being more than 10ppm, Ag+In alkaline environment
Lower to be easy to generate AgOH precipitating, AgOH, which is precipitated and then decomposed, forms silver oxide solid, becomes this part Ag of silver oxide+It cannot send out
Wave activation.Therefore, if AgNO is used alone3, the AgNO in low-temp activation system3Use concentration be necessarily less than or wait
In 10ppm.But at 20 DEG C, the AgNO of 10ppm3The gel breaking time of frozen glue can not be made also to be unable to reach certain pressure break scales pair
The demand of gel breaking time, it is therefore desirable to further shorten gel breaking time, but individual AgNO3It cannot have been reached as activator
To the further purpose for shortening gel breaking time.Only use AgNO3Complex compound is formed with ligand to avoid Ag ion precipitation, ability
Improve Ag ion in fracturing fluid it is effective use concentration.Table 3 is compared with Tables 1 and 2 respectively, it can be seen that the present invention will
AgNO3Soluble complexes are formed with ligand reaction, avoid Ag+AgOH precipitating is generated under alkaline condition；And same concentrations
AgNO3And complex compound, the activation effect of the two are essentially identical.
Table 3 illustrates, individual AgNO3As activator, i.e., under the conditions of no addition ligand, work as AgNO3Concentration increases to
After 10ppm to a certain degree, continue to increase concentration, broken glue effect does not obviously increase.The reason is that Ag ion concentration increases to one
Precipitating can be generated when determining degree, extra Ag becomes precipitating when continuing to increase concentration, petroleum 10ppm always in fracturing fluid
Ag ion plays a role.Compared with Tables 1 and 2, the broken glue effect of the Ag complex compound of concentration 20ppm is substantially better than in table 3
The broken glue effect of 20ppmAg ion.
Table 3 contains various concentration AgNO3Fracturing fluid static gel breaking time at different temperatures
In conclusion the present invention uses Ag+Complex reaction, which is carried out, with ligand forms complex compound as the broken glue activator of low temperature；
The complex compound is water-soluble substances, can be stabilized for a long time in fracturing fluid system；At 50 DEG C, 5ppm activator just can be incited somebody to action
The gel breaking time of frozen glue shortens, and reaches demand of the conventional pressure break scale to gel breaking time, activator dosage is few, significant effect.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of broken glue activator suitable for 20-50 DEG C of reservoir fracturing, which is characterized in that the activator is water-soluble Ag+From
Sub- complex compound.
2. being suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing as described in claim 1, which is characterized in that the activator
What what the ligand B of structure shown in the ligand A or formula II for structure shown in silver ion and formula I was formed be stabilized under alkaline condition
Water soluble complex；
Formula I:
Formula II:
In formula II, R is H or CH3。
3. being suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing as claimed in claim 2, which is characterized in that the activator
The complex compound that the ligand B of structure shown in ligand A or formula II for structure shown in silver nitrate and formula I is formed.
4. being suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing as claimed in claim 3, which is characterized in that the nitric acid
The dosage mass ratio of silver and ligand A or ligand B is 3-5:20-35.
5. being suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing as claimed in claim 3, which is characterized in that the nitric acid
Silver forms the complex compound of molecular structure shown in formula III with ligand A, and silver nitrate and ligand B form the complexing of molecular structure shown in formula IV
Object:
In formula, R is H or CH3。
6. a kind of preparation of the broken glue activator suitable for 20-50 DEG C of reservoir fracturing as described in claim 1-5 any one
Method, which is characterized in that ligand A or B are dissolved in the methanol aqueous solution of the 60-75% containing methanol quality, are heated to 50-70 DEG C,
Adjusting pH is 4-5, and AgNO is added3, stir evenly, adjusting pH with ammonium hydroxide is 7-8 to get to activator.
7. the preparation method suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing, feature exist as claimed in claim 6
In the mass percent of the ligand A or ligand B in methanol aqueous solution is 20-35%.
8. the preparation method suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing, feature exist as claimed in claim 7
In AgNO3Mass percent is 3-5% in methanol aqueous solution.
9. the preparation method suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing, feature exist as claimed in claim 8
In heating temperature is 60 DEG C.
10. the preparation method suitable for the broken glue activator of 20-50 DEG C of reservoir fracturing, feature exist as claimed in claim 8
In using lemon acid for adjusting pH for 4-5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745822A (en) * | 2021-02-03 | 2021-05-04 | 成都劳恩普斯科技有限公司 | Efficient low-temperature gel breaker for polymer fracturing fluid and preparation method of efficient low-temperature gel breaker |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467722A (en) * | 2018-04-17 | 2018-08-31 | 四川申和新材料科技有限公司 | A kind of low temperature breaks glue activator and preparation method thereof |
| CN108587593A (en) * | 2017-12-27 | 2018-09-28 | 中国石油天然气股份有限公司 | Slickwater fracturing fluid for low-temperature reservoir |
| US20180328147A1 (en) * | 2015-03-30 | 2018-11-15 | Baker Hughes, A Ge Company, Llc | Fracturing fluids and methods of treating hydrocarbon formations |
-
2019
- 2019-08-23 CN CN201910781885.6A patent/CN110437818B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180328147A1 (en) * | 2015-03-30 | 2018-11-15 | Baker Hughes, A Ge Company, Llc | Fracturing fluids and methods of treating hydrocarbon formations |
| CN108587593A (en) * | 2017-12-27 | 2018-09-28 | 中国石油天然气股份有限公司 | Slickwater fracturing fluid for low-temperature reservoir |
| CN108467722A (en) * | 2018-04-17 | 2018-08-31 | 四川申和新材料科技有限公司 | A kind of low temperature breaks glue activator and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745822A (en) * | 2021-02-03 | 2021-05-04 | 成都劳恩普斯科技有限公司 | Efficient low-temperature gel breaker for polymer fracturing fluid and preparation method of efficient low-temperature gel breaker |
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