CN109517591A - A kind of high temperature resistant, Low Damage clean fracturing fluid - Google Patents
A kind of high temperature resistant, Low Damage clean fracturing fluid Download PDFInfo
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Abstract
The present invention relates to a kind of high temperature resistants, Low Damage clean fracturing fluid, it is to be prepared via a method which: high temperature resistant Gemini surface active agent is mixed with alcohol auxiliary agent, is added to the water, and is uniformly mixed, then counter ion salt is added, is uniformly mixed up to high temperature resistant, Low Damage clean fracturing fluid；The concentration of high temperature resistant Gemini surface active agent is 1.5-5.5% in high temperature resistant, Low Damage clean fracturing fluid, and counter ion salinity is 0.2-2.2%, and alcohol assistant concentration is 1-5%.Fracturing fluid of the invention is using high temperature resistant Gemini surface active agent as thickening agent, at 130 DEG C, 170s‑1Under shear rate, viscosity can achieve 30mPas, temperature tolerance is good, with broken zero residue of glue, reservoir damage is low, ultralow leak-off, characteristic resistant to high temperature, solve the problems, such as that conventional clean fracturing fluid easily forms precipitating when temperature is lower, facilitate live use, can satisfy the requirement in high temperature oil gas field.
Description
Technical field
The present invention relates to a kind of high temperature resistants, Low Damage clean fracturing fluid, belong to oil field fracturing technical field.
Background technique
As continually developing for high benefit oil gas field is increasingly reduced with high-grade oil reservoir, demand of the countries in the world to petroleum
Swift and violent to increase, the troop of domestic and international petroleum exploration & development is all to hypotonic, special hypotonic, viscous crude oil gas field and small reserves side
Border oil gas field etc. marches.Reservoir fracturing improvement becomes the key for improving oil recovery factor, and hydraulic fracturing is transformed into low-permeability oil
Gas reservoir improves the key of oil recovery factor, is widely used in oil field prospecting and exploitation.Routine fracturing fluid system is main at present
It is with high molecular polymer (natural plant, as guanidine glue and its derivative, cellulose pressure, such as carboxymethyl cellulose, synthesis gather
Close object, such as polyacrylamide) fracturing fluid system as thickening agent, but conventional fracturing fluid during the row of returning due to broken glue
Very major injury can be caused to oil-gas reservoir permeability by being not thorough.With the exploitation of unconventional shale gas, fine and close oil etc., conventional reservoir
Transformation has been unable to meet the requirement of current fracturing reform, and therefore, the research and development of high-performance fracturing fluid become current untraditional reservoir
Urgent problem to be solved in reservoir reconstruction.
Clean fracturing fluid is also referred to as viscoelastic surfactant fracturing fluid (VES), is a kind of based on Viscoelastic surfactant
The solution of agent has the advantages that row of returning is rapid and thorough, injury is low, and solid-carrying performance is good, and vena caval filter performance is good, solves routine
Fracturing fluid system breaks the halfway defect of glue.
As oil field is gradually to deep layer, the transfer of high temperature, Low permeable oil and gas reservoirs, fracturing methods well is mostly high temperature deep well, pressure
The temperature tolerance for splitting liquid system just becomes technical problem urgently to be resolved at present.
About the research of clean fracturing fluid, there are reports at present, for example, with stearic acid, N, TMSDMA N dimethylamine base propylamine and
1,3- bis- chloro- 2- propyl alcohol is Material synthesis Gemini surface active agent, and synthesized Gemini surface active agent is formed with hydrochloric acid again
Acid clean fracturing fluid；But there are the following shortcomings for the acidic fracturing fluid: performance is unstable, and it is heavy easily to be formed when temperature is lower
It forms sediment, scene is very inconvenient when using；In addition, the heat resistance of the clean fracturing fluid is not high, at 105 DEG C, the fracturing fluid viscosity drops
To 30mPaS hereinafter, being unable to satisfy the requirement in high temperature oil gas field,
For another example anionic clean fracturing fluid, Recent study is active, is that the following Low Damage VES clean fracturing fluid is researched and developed
One important directions.But the VES clean fracturing liquid system heat resistance studied at present generally can only achieve 90-100 DEG C, hardly possible
To be applied in 120 DEG C of high-temperature stratum.
Summary of the invention
For the above the deficiencies in the prior art, the present invention provides a kind of high temperature resistant, Low Damage clean fracturing fluid, the fracturing fluid
At 130 DEG C, 170s-1Under shear rate, viscosity can achieve 30mPas, and temperature and shearing sustainability is good, have broken glue zero residual
Slag, reservoir damage be low, ultralow leak-off, characteristic resistant to high temperature.
The present invention is achieved through the following technical solutions:
A kind of high temperature resistant, Low Damage clean fracturing fluid, are prepared via a method which:
1) alkyl phenol and halogenated hydrocarbons carry out nucleophilic displacement of fluorine and generate bis ether intermediate, and bis ether intermediate progress sulfonation, neutralization are anti-
It answers, removes solvent, washing is recrystallized to give high temperature resistant Gemini surface active agent；
2) high temperature resistant Gemini surface active agent is mixed with alcohol auxiliary agent, is added to the water, is uniformly mixed, is then added
Counter ion salt is uniformly mixed up to high temperature resistant, Low Damage clean fracturing fluid；
The concentration of high temperature resistant Gemini surface active agent is 1.5-5.5%, counter ion in high temperature resistant, Low Damage clean fracturing fluid
Salinity is 0.2-2.2%, and alcohol assistant concentration is 1-5%.
It is preferred according to the present invention, the concentration of high temperature resistant Gemini surface active agent in high temperature resistant, Low Damage clean fracturing fluid
For 1.5-4.5%, counter ion salinity is 0.6-1.2%, and alcohol assistant concentration is 2-3%.
It is preferred according to the present invention, the concentration of high temperature resistant Gemini surface active agent in high temperature resistant, Low Damage clean fracturing fluid
It is 2.5%, counter ion salinity is 1.0%, and alcohol assistant concentration is 3%.
Preferred according to the present invention, counter ion salt is sodium salicylate.
Preferred according to the present invention, alcohol auxiliary agent is one of n-octyl alcohol, Decanol or n-dodecanol, further preferably
, alcohol auxiliary agent is Decanol.
A preferred scheme according to the present invention, in step (1), alkyl phenol and halogenated hydrocarbons carry out nucleophilic displacement of fluorine and generate bis ether
The specific method is as follows for intermediate:
It is stirred evenly after alkyl phenol is mixed with cetyl trimethylammonium bromide, NaOH aqueous solution, is heated to 60-80
DEG C, halogenated hydrocarbons is added, is continuously heating to 90-100 DEG C, reacts 2-6h, it is cooling after ether extract, during extract liquor is washed with water to
Property, then solvent evaporated, obtains bis ether intermediate, and the alkyl phenol is the alkyl phenol of linear carbon chain C8-C12.
Preferred according to the present invention, the dosage of cetyl trimethylammonium bromide is the 0.05-0.1% of alkyl phenol quality；
The molar ratio of alkyl phenol and halogenated hydrocarbons is 1-4:1；The mass concentration 15-25% of NaOH aqueous solution, alkyl phenol and NaOH aqueous solution
Molar ratio be 1:4-6, the halogenated hydrocarbons be dibromobutane.
A preferred scheme according to the present invention, in step (1), bis ether intermediate sulfonation is specific as follows:
Chlorosulfonic acid is dissolved in anhydrous methylene chloride, is then added in the bis ether intermediate of anhydrous methylene chloride dissolution, in room
Temperature is lower to react 6-10h, recycles hydrogen chloride simultaneously in reaction process.
Preferred according to the present invention, the molar ratio of chlorosulfonic acid and bis ether intermediate is 1-4:1, bis ether intermediate and anhydrous two
The molar ratio of chloromethanes is 1:12-16, the mass ratio 1:2-5 of chlorosulfonic acid and anhydrous methylene chloride.
A preferred scheme according to the present invention, in step (1), the neutralization reaction is molten with the ethyl alcohol of sodium hydroxide
Liquid neutralizes, and the ethanol solution of sodium hydroxide is dissolved in 50mL ethyl alcohol for 5gNaOH and obtains, and being neutralized to reaction product pH=7 terminates, and washes
It washs then to filter, obtained filtrate is recrystallized with ethyl alcohol, and finished product is obtained after drying with acetone washing.
Beneficial effects of the present invention and advantage:
1, fracturing fluid of the invention is using high temperature resistant Gemini surface active agent as thickening agent, at 130 DEG C, 170s-1Shearing speed
Under rate, viscosity can achieve 30mPas, and temperature tolerance is good, have low broken zero residue of glue, reservoir damage, ultralow leak-off, high temperature resistant
Characteristic, solve the problems, such as conventional clean fracturing fluid when temperature is lower easily formed precipitating, facilitate live use, can satisfy
The requirement in high temperature oil gas field；
2, traditional fracturing fluid would generally use kind of an additive, and its inorganic salt content is high, cause scene with liquid workload
Greatly, the time is long, at high cost, and clean fracturing fluid of the invention only needs 3 kinds of substances in process for preparation, simple with liquid process,
It is easy to use, it is at low cost；
3, fracturing fluid solid-carrying performance of the invention is good；Glue can be broken by meeting stratum oil and water, without adding gel breaker, breaking glue solution
Viscosity is low, no residue, no filter cake, to bottom fanout free region.
Detailed description of the invention
Fig. 1 is the Low Damage clean fracturing fluid heat resistance figure of embodiment 1.
Specific embodiment
To further illustrate the present invention, it is exemplified below specific embodiment, but institute's protection scope of the present invention is not limited only to this.
Embodiment 1
A kind of high temperature resistant, Low Damage clean fracturing fluid, are prepared via a method which:
1) preparation of heatproof Gemini surface active agent:
By dodecylphenol be placed in equipped with mechanical stirring, reflux condensing tube three-necked flask in, be added dodecylphenol matter
0.07% cetyl trimethylammonium bromide and mass concentration of amount are 20%NaOH aqueous solution 100mL stirring, and are heated to
75 DEG C, the ratio for being 1:2.02 according to the molar ratio of dibromobutane and dodecylphenol pipettes dibromobutane and reaction system is added,
Continue to be heated to 100 DEG C, react 4h, after system is cooling, ether is added by several times into system and is extracted, extract liquor is used
Water washing is washed till neutrality, then uses Rotary Evaporators solvent evaporated, can obtain bis ether intermediate；
Bis ether intermediate is placed in the three-necked flask equipped with hydrogen chloride absorption device, and the anhydrous dichloromethane of 50mL is added
It is anhydrous to be dissolved in 30mL by alkane, magnetic agitation, the ratio for being 2.02:1 according to the molar ratio of chlorosulfonic acid and bis ether intermediate for chlorosulfonic acid
Methylene chloride instills reaction system in 1h at room temperature, the reaction was continued 8h,
Neutralized with the ethanol solution of sodium hydroxide, solvent evaporated, with acetone washing product, filtering, by filtrate with ethyl alcohol into
Row recrystallization, dries to obtain Gemini surface active agent；
2) preparation of clean fracturing fluid:
High temperature resistant Gemini surface active agent is mixed with n-dodecanol, is added to the water, is uniformly mixed, be then added
Sodium salicylate is uniformly mixed up to high temperature resistant, Low Damage clean fracturing fluid；
The concentration of high temperature resistant Gemini surface active agent is 2.5% in high temperature resistant, Low Damage clean fracturing fluid, and n-dodecanol is dense
Degree is 3%, sodium salicylate 1.0%.
Experimental example 1:
1, using high temperature rheometer, the Low Damage clean fracturing fluid heat resistance of embodiment 1, test result such as Fig. 1 are evaluated
It is shown.
When fracturing liquid ties up to 130 DEG C -140 DEG C, viscosity can achieve 30mPas, and temperature tolerance is good.
2, the Low Damage clean fracturing fluid for measuring embodiment 1 under different temperatures takes sand sinking speed.
Fracturing fluid system is added in the intermediate receptacle with visual window, density 3.31g/cm is added3, partial size 40-60 mesh
Sand grains, it is closed, heating.The sinking speed of sand grains is observed by visual window at different temperatures, test result is shown in Table 1:
1 fracturing fluid of table takes sand sinking speed
| Temperature, DEG C | 40 | 60 | 80 | 100 | 120 |
| Fracturing fluid system viscosity, mPa.s | 194 | 178 | 170 | 96 | 36 |
| Average settlement speed, cm/min | 0.35 | 0.30 | 0.41 | 1.16 | 3.41 |
It is the rate of settling of near perfect less than 0.5cmmin-1；It is unacceptable sedimentation greater than 5cmmin-1
Rate；Between 0.5-5cmmin-1, between be then the preferable rate of settling.
When in 80 DEG C, it is very good that fracturing fluid takes sand suspension effect.Under the conditions of 120 DEG C, sand fallout fast speed, but
Still meet and takes sand suspension requirement.
3, the fracturing fluid static filtration of the Low Damage clean fracturing fluid of embodiment 1 under different temperatures, test result are measured
It is shown in Table 2:
2 clean fracturing fluid leak-off of table
| Temperature, DEG C | Spurt loss volume, mL/m3 | Leak-off slope, L/min | Leakoff coefficent, m/min1/2 |
| 40 | 0.01 | 0.12 | 1.1×10-4 |
| 80 | 0.005 | 0.23 | 1.9×10-4 |
| 120 | 0.002 | 0.5 | 2.2×10-4 |
Clean fracturing fluid viscosity is high, and filter loss is less, and leakoff coefficent is 10-4The order of magnitude, it is static with hydroxypropyl guar system
Leakoff coefficent is compared, and an order of magnitude can be reduced.
4, when kerosene, fracturing fluid and kerosene volume ratio 10:1 being added into the fracturing fluid of embodiment 1, breaking glue solution after 40min
Viscosity is lower than 5mPa.s, and it is good to break glue responsiveness.
5, kerosene is added into the fracturing fluid of embodiment 1 and breaks glue, measure the content of fracturing fluid residue after breaking gel.
Residue content is 0mg/L to the clean fracturing liquid system of preparation after breaking gel, and fracturing fluid residue content is 0mg/L, can be broken
Glue is entirely without residue.
6, breaking glue solution under different permeabilities is measured to the injury situation of rock core, and test result is shown in Table 3.
3 clean fracturing fluid of table tests (90 DEG C) to matrix core damage
Clean fracturing fluid breaking glue solution is to core permeability injury rate < 12%, to the permeability retention rate > 88% of rock core.
It is smaller to the injury of reservoir after illustrating fracturing liquid rubber-breaking, meet Low Damage requirement.
Comparative example 1
A kind of clean fracturing fluid, component with embodiment 1, unlike, which is to use butylphenol
Dodecylphenol is replaced, obtained clean fracturing fluid carries out carrying out high-temperature viscosity comparison with embodiment 1.
Comparative example 2
A kind of clean fracturing fluid, component with embodiment 1, unlike, which is to use amylic phenol
Dodecylphenol is replaced, obtained clean fracturing fluid carries out carrying out high-temperature viscosity comparison with embodiment 1.
Comparative example 3
A kind of clean fracturing fluid, component with embodiment 1, unlike, which is with heptyl phenol
Dodecylphenol is replaced, obtained clean fracturing fluid carries out carrying out high-temperature viscosity comparison with embodiment 1.
Experimental example 2:
Using high temperature rheometer, the Low Damage clean fracturing fluid of embodiment 1 and the heat resistance of comparative example 1-3 are evaluated,
Viscosity is as follows when fracturing liquid ties up to 130 DEG C:
Table 4
| Project | Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Fracturing fluid system viscosity, mPa.s | 36 | 18 | 20 | 21 |
Embodiment 2
A kind of high temperature resistant, Low Damage clean fracturing fluid, with embodiment 1, the difference is that:
The concentration of high temperature resistant Gemini surface active agent is 4.5% in high temperature resistant, Low Damage clean fracturing fluid, and n-dodecanol is dense
Degree is 2.5%, sodium salicylate 1.2%.
Claims (10)
1. a kind of high temperature resistant, Low Damage clean fracturing fluid, are prepared via a method which:
1) alkyl phenol and halogenated hydrocarbons carry out nucleophilic displacement of fluorine and generate bis ether intermediate, and bis ether intermediate carries out sulfonation, neutralization reaction, goes
Except solvent, washing is recrystallized to give high temperature resistant Gemini surface active agent；
2) high temperature resistant Gemini surface active agent is mixed with alcohol auxiliary agent, is added to the water, is uniformly mixed, be then added instead from
Alite is uniformly mixed up to high temperature resistant, Low Damage clean fracturing fluid；
The concentration of high temperature resistant Gemini surface active agent is 1.5-5.5% in high temperature resistant, Low Damage clean fracturing fluid, and counter ion salt is dense
Degree is 0.2-2.2%, and alcohol assistant concentration is 1-5%.
2. clean fracturing fluid according to claim 1, which is characterized in that resistance to height in high temperature resistant, Low Damage clean fracturing fluid
The concentration of warm Gemini surface active agent is 1.5-4.5%, and counter ion salinity is 0.6-1.2%, and alcohol assistant concentration is 2-3%.
3. clean fracturing fluid according to claim 1, which is characterized in that resistance to height in high temperature resistant, Low Damage clean fracturing fluid
The concentration of warm Gemini surface active agent is 2.5%, and counter ion salinity is 1.0%, and alcohol assistant concentration is 3%.
4. clean fracturing fluid according to claim 1, which is characterized in that counter ion salt is sodium salicylate.
5. clean fracturing fluid according to claim 1, which is characterized in that alcohol auxiliary agent is n-octyl alcohol, Decanol or positive 12
One of alcohol, it is further preferred that alcohol auxiliary agent is Decanol.
6. clean fracturing fluid according to claim 1, which is characterized in that in step (1), alkyl phenol and halogenated hydrocarbons carry out parent
Core replaces generation bis ether intermediate, and the specific method is as follows:
It is stirred evenly after alkyl phenol is mixed with cetyl trimethylammonium bromide, NaOH aqueous solution, is heated to 60-80 DEG C, adds
Enter halogenated hydrocarbons, be continuously heating to 90-100 DEG C, react 2-6h, ether extracts after cooling, and extract liquor is washed with water to neutrality, then
Solvent evaporated, obtains bis ether intermediate, and the alkyl phenol is the alkyl phenol of linear carbon chain C8-C12.
7. clean fracturing fluid according to claim 1, which is characterized in that in step (1), cetyl trimethylammonium bromide
Dosage be alkyl phenol quality 0.05-0.1%；The molar ratio of alkyl phenol and halogenated hydrocarbons is 1-4:1；The quality of NaOH aqueous solution
The molar ratio of concentration 15-25%, alkyl phenol and NaOH aqueous solution is 1:4-6, and the halogenated hydrocarbons is dibromobutane.
8. clean fracturing fluid according to claim 1, which is characterized in that in step (1), the sulfonation of bis ether intermediate is specifically such as
Under:
Chlorosulfonic acid is dissolved in anhydrous methylene chloride, is then added in the bis ether intermediate of anhydrous methylene chloride dissolution, at room temperature
6-10h is reacted, recycles hydrogen chloride simultaneously in reaction process.
9. clean fracturing fluid according to claim 1, which is characterized in that in step (1), chlorosulfonic acid and bis ether intermediate
Molar ratio is 1-4:1, and the molar ratio of bis ether intermediate and anhydrous methylene chloride is 1:12-16, chlorosulfonic acid and anhydrous methylene chloride
Mass ratio 1:2-5.
10. clean fracturing fluid according to claim 1, which is characterized in that in step (1), in step (1), it is described in
With reaction to be neutralized with the ethanol solution of sodium hydroxide, the ethanol solution of sodium hydroxide is dissolved in 50mL ethyl alcohol for 5gNaOH and obtains,
Being neutralized to reaction product pH=7 terminates, and washs then to filter with acetone washing, and obtained filtrate is recrystallized with ethyl alcohol,
Finished product is obtained after drying.
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| CN111073626A (en) * | 2019-12-30 | 2020-04-28 | 陕西省石油化工研究设计院 | Clean fracturing fluid for low-permeability, high-temperature-resistant and high-pressure-resistant reservoir and preparation method thereof |
| CN114085171A (en) * | 2021-12-03 | 2022-02-25 | 中国石油大学(华东) | Surfactant for natural gas hydrate clean fracturing fluid and preparation method thereof |
| CN114674640A (en) * | 2022-04-12 | 2022-06-28 | 西南石油大学 | Experimental method for evaluating damage of fracturing fluid to dense gas reservoir matrix |
| CN115044384A (en) * | 2022-05-30 | 2022-09-13 | 中国石油大学(华东) | Anionic-nonionic gemini surfactant for natural gas hydrate clean fracturing fluid and preparation method thereof |
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| CN111073626A (en) * | 2019-12-30 | 2020-04-28 | 陕西省石油化工研究设计院 | Clean fracturing fluid for low-permeability, high-temperature-resistant and high-pressure-resistant reservoir and preparation method thereof |
| CN115746818A (en) * | 2021-09-03 | 2023-03-07 | 中国石油天然气集团有限公司 | Low-fluid-loss recyclable fracturing fluid and preparation method and recycling method thereof |
| CN114085171A (en) * | 2021-12-03 | 2022-02-25 | 中国石油大学(华东) | Surfactant for natural gas hydrate clean fracturing fluid and preparation method thereof |
| CN114674640A (en) * | 2022-04-12 | 2022-06-28 | 西南石油大学 | Experimental method for evaluating damage of fracturing fluid to dense gas reservoir matrix |
| CN114674640B (en) * | 2022-04-12 | 2024-07-02 | 西南石油大学 | Experimental method for evaluating damage of fracturing fluid to tight gas reservoir matrix |
| CN115044384A (en) * | 2022-05-30 | 2022-09-13 | 中国石油大学(华东) | Anionic-nonionic gemini surfactant for natural gas hydrate clean fracturing fluid and preparation method thereof |
| CN115044384B (en) * | 2022-05-30 | 2024-02-13 | 中国石油大学(华东) | Anionic-nonionic amphoteric gemini surfactant for natural gas hydrate clean fracturing fluid and preparation method thereof |
| CN115286526A (en) * | 2022-07-15 | 2022-11-04 | 山西蓝焰煤层气集团有限责任公司 | Surfactant and preparation method and application thereof |
| CN115286526B (en) * | 2022-07-15 | 2023-10-13 | 山西蓝焰煤层气集团有限责任公司 | Surfactant and preparation method and application thereof |
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