CN108822826A - A kind of low corrosion green crosslinked acid fracturing fluid and the preparation method and application thereof - Google Patents
A kind of low corrosion green crosslinked acid fracturing fluid and the preparation method and application thereof Download PDFInfo
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- 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
- C09K8/62—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
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
Abstract
The present invention relates to a kind of low corrosion green crosslinked acid fracturing fluids and the preparation method and application thereof, and material quality percentage is as follows：Organic acid 15~20%, polymer thickening agent 0.6~1.2%, organic zirconium crosslinker 1.0~5.0%, gel breaker 0.01~0.05%, remaining is water, and the sum of each component mass percent is absolutely；Organic acid is lactic acid and gluconic acid is (1-2) in molar ratio:The mixed acid of the ratio mixing of (1-2)；The main body sour component that low corrosion green crosslinked acid fracturing fluid of the invention uses is weak organic acid; weak organic acid is small to the corrosion strength of pit shaft and equipment; it can be with effective protection pit shaft and relevant device; the rate of corrosion for reducing equipment extends service life, while avoiding the pollution to environment; reduce the injury to staff; the calcium salt solubility with higher that organic acid generates, greatly reduces calcium precipitate amount, greatly reduces the secondary pollution to stratum.
Description
Technical field
The present invention relates to a kind of low corrosion green crosslinked acid fracturing fluids and the preparation method and application thereof, belong to fracturing fluid technology
Field.
Background technique
Acid-fracture technology refers under conditions of bottom pressure is higher than formation fracture pressure, squeezes acid fracturing and breaks stratum, is formed
Man-made fracture, injection acid solution, which performs etching in crack with wall surface, reacts, so that crack can not be closed completely after construction,
To promote stratum flow conductivity.For currently used ACID FRACTURING TECHNOLOGY, acidification working solution passes through in the construction process
Pit shaft is injected into stratum, is acidified contact of the working solution with pit gear and is inevitable.Therefore, acid solution is to pit gear
Corrosion is the problem of can not avoiding at present.
Deep ACID FRACTURING TECHNOLOGY and common acid fracturing are essentially the same, and difference is the working solution for selecting filter loss low, it is therefore an objective to obtain
Obtain acid-etched fracture longer than common acid fracturing.Cross-linked acid refers to acid fluid system being crosslinked by thickening agent and mating crosslinking agent, shape
At network gel structure, system viscosity is significantly improved, to reduce filter loss, acid fracturing system has been used as to be made extensively at present
With.
Chinese patent literature CN104403658A discloses a kind of high temperature resistant crosslinking acid fluid system and preparation method thereof, the friendship
Join acid system by mass percentage by hydrochloric acid (5-25wt%), polymer thickening agent (0.5-1.2wt%), chelating titanium crosslinkers
(0.2-0.5wt%), water composition, wherein the polymer thickening agent is acrylamide-methylacryoyloxyethyl trimethyl
Ammonium chloride copolymer, monomer mole ratio 8:3~15:3；The chelating titanium crosslinkers be titanium sulfate, titanium chloride, Titanium Nitrate,
Acetic acid titanium, which is dissolved in water, has chelating agent reaction to be made, and the system heatproof is up to 160-190 DEG C.
Chinese patent literature CN104073237A discloses a kind of high temperature resistant ground surface crosslinking acid acid solution and preparation method thereof, should
Acid fluid system is handed over by hydrochloric acid (15-28wt%), polyacrylamide polymer (0.4-1.0wt%), aldehydes by mass percentage
Join agent (0.1-0.5wt%), Phenolic crosslinkers (0.05-0.25wt%), ammonium persulfate (0.01-0.1wt%), water composition.It should
The crosslinking agent toxicity that system uses is low, and preparation process is simple, at low cost, but temperature tolerance is not strong, and only 120 DEG C.
Most of existing crosslinked acid fracturing fluid is using hydrochloric acid as acidification main acid, using having for thickening agent and crosslinking agent
Effect crosslinking, hydrochloric acid should not be underestimated to the corrosion of pit gear as strong acid, and hydrochloric acid is volatile, will cause pollution to environment；And
And the temperature tolerance for the thickening agent, crosslinking agent having is poor, toxicity is big, therefore, the generally existing corrosivity of current crosslinked acid fracturing fluid with
The defect that temperature tolerance, leak-off cannot get both.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provide a kind of low corrosion green crosslinked acid fracturing fluid and preparation method thereof with
Using, the main scarce filling which overcomes the corrosivity of existing cross-linked acid strong, and take into account the temperature tolerance of system, leak-off
Property, toxicity, volatility.Main body acid solution used in the present invention is green organic acid, small to the corrosivity of pit shaft, not volatile,
And main acid reacts with carbonate rock and does not generate secondary precipitation, it is small to formation damage.Polymer thickening agent and crosslinking agent can be in acid
It is crosslinked in liquid, and breaks the glue thoroughly easy row of returning after reacting.
A kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Remaining is water, and the sum of each component mass percent is absolutely.
Preferred according to the present invention, the organic acid is lactic acid and gluconic acid is (1-2) in molar ratio:(1-2's)
The mixed acid of ratio mixing.
Preferred according to the present invention, the polymer thickening agent is partially hydrolyzed polyacrylamide (PHPA) class thickening agent.
It is further preferred that the polymer thickening agent is by acrylamide (AM) and 2- acrylamido -2- methyl -
Propanesulfonate (AMPS) is 2.0~3.0 in molar ratio:1 ratio is copolymerized, and the molecular weight of polymer thickening agent is 600~
10000000.
It is preferred according to the present invention, the organic zirconium crosslinker be by zirconium oxychloride, isopropanol meltage it is water-soluble
Xie Hou, 3~4h of water-bath at a temperature of 50~55 DEG C, during which intermittence stirs, and adds lactic acid and xylitol reaction 10-
It is made after 20min.
Preferred according to the present invention, zirconium oxychloride, water, isopropanol, lactic acid and xylitol mass ratio are (0.8-1.2)：(1-
1.4)：(2-2.8)：(1-1.4)：(0.0-0.03)；It is highly preferred, zirconium oxychloride, water, isopropanol, lactic acid and xylitol matter
Amount is than being 1:1.25:2.5:1.25:0.02.
According to the present invention, the gel breaker is the capsule breaker made of potassium peroxydisulfate.
A currently preferred technical solution,
A kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Remaining is water, and the sum of each component mass percent is absolutely.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent being added in the mixed liquor of step (1), stirring is to being completely dissolved, after standing 20-28h,
In proportion, crosslinking agent and gel breaker is added, stirs evenly, obtains the low corrosion green crosslinked acid fracturing fluid.
Preferred according to the present invention, the speed of agitator after polymer thickening agent is added in step (2) is 400-500r/min,
Gel breaker is added after crushing, and the speed of agitator after crosslinking agent and gel breaker is added is 600-700r/min, stirs evenly and is placed on
Dry 4h in 90 DEG C of baking ovens.
A kind of application of low corrosion green crosslinked acid fracturing fluid, in carbonate formation Depth Acid Fracturing technique.
The principle of the present invention is as follows：
Improve the principle of marl solubility：
Main acid is organic acid in low corrosion green crosslinked acid fracturing fluid system of the invention, the calcium salt tool that organic acid generates
There is higher solubility, action principle depends on the synergistic effect of lactic acid and gluconic acid dissolving calcium, when lactic acid is used alone,
The solubility of the calcium lactate precipitate of generation is lower, and after gluconic acid is added, lactic acid, gluconic acid and calcium generate lactic acid glucose
Sour calcium, such as following formula I, lactic acid calcium gluconate is constituted for a kind of two sour ligands by calcium ion complexing lactic acid and gluconic acid
The solubility of compound, this compound is larger；Therefore, the calcium salt solubility with higher that organic acid of the invention generates,
Greatly reduce calcium precipitate amount.
Green crosslinking acid system improves the principle of effective distance of live acid：
Organic acid used in the present invention belongs to weak acid system, is in aqueous solution incomplete ionization state, with anti-with rock
Hydrogen ion should constantly be consumed and organic acid gradually release hydrogen ions, to be effectively reduced acid-rock reaction speed；On the other hand, originally
The organic zirconium crosslinker of invention is capable of providing a kind of polynuclear hydroxy bridge complex ion, can hand over the functional group in thickening agent molecular structure
Connection increases substantially system viscosity, can not only reduce acid solution so that acid fluid system be promoted to form the frozen glue of space network
Leak-off, and hydrogen ion passes through the frozen glue and rock contact of space network, significantly reduces hydrionic mass transfer velocity, thus
Reduce acid-rock reaction speed.The present invention reduces acid-rock reaction speed in terms of above-mentioned two, when the reduction of acid-rock reaction speed, acid solution body
System is obviously prolonged from the time that active acid becomes residual acid, so that the EFFECTIVE RANGE that acid solution flows in the earth formation increases,
Available longer acid-etched fracture.
Compared with prior art, the beneficial effects of the invention are as follows：
1. the main body sour component that low corrosion green crosslinked acid fracturing fluid of the invention uses is weak organic acid, weak organic acid pair
The corrosion strength of pit shaft and equipment is small, can reduce the rate of corrosion of equipment, extending makes with effective protection pit shaft and relevant device
With the service life, while the pollution to environment is avoided, reduces the injury to staff.
2. the main acid that low corrosion green crosslinked acid fracturing fluid of the invention uses is organic acid, the calcium salt of organic acid generation
Solubility with higher greatly reduces calcium precipitate amount, greatly reduces the secondary pollution to stratum.
3. main body sour component of the present invention is weak organic acid, in aqueous solution incomplete ionization；Simultaneously using crosslinking agent with it is thick
The mode that agent is crosslinked in acid solution, the viscosity for increasing system reduce filter loss, and acid solution body can be improved in the two synergistic effect
The operating distance of system in the earth formation, available longer acid-etched fracture.
4. the present invention uses capsule breaker, can during acid fracturing opportunity more appropriate discharge break glue to greatest extent
Agent keeps brokenly glue thorough, the liquid easily row of returning after reaction.
Specific embodiment
Below by specific embodiment, the invention will be further described, but is not limited only to following instance.
All percentages are mass percent in embodiment, and product used in embodiment is commercial product.
Embodiment 1：
A kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Organic acid 15%, polymer thickening agent 1.0%, organic zirconium crosslinker 4.0%, gel breaker 0.03%, remaining is water.
Organic acid is lactic acid and gluconic acid is 1 in molar ratio:The mixed acid of 1 ratio mixing.
Polymer thickening agent is massaged by acrylamide (AM) and 2- acrylamido -2- methyl-propanesulfonic acid sodium (AMPS)
You are than being 2.0~3.0:1 ratio is copolymerized, and the molecular weight of polymer thickening agent is 600~10,000,000.
Organic zirconium crosslinker is prepared as follows to obtain：12.0g zirconium oxychloride and 30.0g isopropanol are dissolved in
In 15.0g distilled water, with 190r/min stir to it is complete it is molten after, pour into three-necked flask, access reflux condensate device, fixing 50 DEG C
At a temperature of after water-bath is stirred to react 3h with 400r/min, 15.0g lactic acid and 0.25g xylitol is added, the reaction was continued 15min is to molten
Liquid uniformly to get arrive organic zirconium crosslinker.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), is at the uniform velocity stirred with 400r/min to being completely dissolved
Afterwards, after standing for 24 hours, in proportion, crosslinking agent and gel breaker is added, is added after capsule breaker is pulverized, at the uniform velocity with 600r/min
After stirring 35min, it is put in 4h in 90 DEG C of baking ovens, obtains the low corrosion green crosslinked acid fracturing fluid.
The breaking glue solution of the crosslinked acid fracturing fluid of the present embodiment is uniform, is in khaki, invisible residue, under the conditions of 30 DEG C
Viscosity is 5mPas.Illustrate brokenly that glue works well, it is low to hydrocarbon contamination extent of injury.
The crosslinked acid fracturing fluid of the present embodiment is reacted with marble has good slow speed effect, reacts corrosion rate after 10h
Only 60% or so.
The crosslinked acid fracturing fluid of the present embodiment is in 140 DEG C, shear rate 170s-1Under conditions of shear 1h after, viscosity is
90mPas illustrates that temperature tolerance is good.
Embodiment 2：
A kind of low corrosion green crosslinked acid fracturing fluid, with embodiment 1.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), is at the uniform velocity stirred with 450r/min to being completely dissolved
Afterwards, after standing for 24 hours, in proportion, crosslinking agent and gel breaker is added, is added after capsule breaker is pulverized, at the uniform velocity with 650r/min
After stirring 35min, it is put in 4h in 90 DEG C of baking ovens, obtains the low corrosion green crosslinked acid fracturing fluid.
The breaking glue solution of the crosslinked acid fracturing fluid of the present embodiment is uniform, is in khaki, invisible residue, under the conditions of 30 DEG C
Viscosity is 6mPas.Illustrate brokenly that glue works well, it is low to hydrocarbon contamination extent of injury.
The crosslinked acid fracturing fluid of the present embodiment is reacted with marble has good slow speed effect, reacts corrosion rate after 10h
Only 65% or so.
The crosslinked acid fracturing fluid of the present embodiment is in 140 DEG C, shear rate 170s-1Under conditions of shear 1h after, viscosity is
93mPas illustrates that temperature tolerance is good.
Embodiment 3：
A kind of low corrosion green crosslinked acid fracturing fluid, with embodiment 1.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), is at the uniform velocity stirred with 500r/min to being completely dissolved
Afterwards, after standing for 24 hours, in proportion, crosslinking agent and gel breaker is added, is added after capsule breaker is pulverized, at the uniform velocity with 600r/min
After stirring 35min, it is put in 4h in 90 DEG C of baking ovens, obtains the low corrosion green crosslinked acid fracturing fluid.
The breaking glue solution of the crosslinked acid fracturing fluid of the present embodiment is uniform, is in khaki, invisible residue, under the conditions of 30 DEG C
Viscosity is 8mPas.Illustrate brokenly that glue works well, it is low to hydrocarbon contamination extent of injury.
The crosslinked acid fracturing fluid of the present embodiment is reacted with marble has good slow speed effect, reacts corrosion rate after 10h
Only 55% or so.
The crosslinked acid fracturing fluid of the present embodiment is in 140 DEG C, shear rate 170s-1Under conditions of shear 1h after, viscosity is
88mPas illustrates that temperature tolerance is good.
Embodiment 4：
A kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Organic acid 15%, polymer thickening agent 0.8%, organic zirconium crosslinker 3.0%, gel breaker 0.03%, remaining is water.
Organic acid, polymer thickening agent, organic zirconium crosslinker are the same as embodiment 1.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), is at the uniform velocity stirred with 400r/min to being completely dissolved
Afterwards, after standing for 24 hours, in proportion, crosslinking agent and gel breaker is added, is added after capsule breaker is pulverized, at the uniform velocity with 600r/min
After stirring 35min, it is put in 4h in 90 DEG C of baking ovens, obtains the low corrosion green crosslinked acid fracturing fluid.
The breaking glue solution of the crosslinked acid fracturing fluid of the present embodiment is uniform, is in khaki, invisible residue, under the conditions of 30 DEG C
Viscosity is 9mPas.Illustrate brokenly that glue works well, it is low to hydrocarbon contamination extent of injury.
The crosslinked acid fracturing fluid of the present embodiment is reacted with marble has good slow speed effect, reacts corrosion rate after 10h
Only 55% or so.
The crosslinked acid fracturing fluid of the present embodiment is in 140 DEG C, shear rate 170s-1Under conditions of shear 1h after, viscosity is
85mPas illustrates that temperature tolerance is good.
Embodiment 5：
A kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Organic acid 20%, thickening agent 1.2%, organic zirconium crosslinker 4.0%, gel breaker 0.03%, remaining is water.
Organic acid, polymer thickening agent, organic zirconium crosslinker are the same as embodiment 1.
The preparation method of low corrosion green crosslinked acid fracturing fluid, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, organic acid is then added while stirring
In gluconic acid, stir evenly, obtain mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), is at the uniform velocity stirred with 400r/min to being completely dissolved
Afterwards, after standing for 24 hours, in proportion, crosslinking agent and gel breaker is added, is added after capsule breaker is pulverized, at the uniform velocity with 600r/min
After stirring 35min, it is put in 4h in 90 DEG C of baking ovens, obtains the low corrosion green crosslinked acid fracturing fluid.
The breaking glue solution of the crosslinked acid fracturing fluid of the present embodiment is uniform, is in khaki, invisible residue, under the conditions of 30 DEG C
Viscosity is 10mPas.Illustrate brokenly that glue works well, it is low to hydrocarbon contamination extent of injury.
The crosslinked acid fracturing fluid of the present embodiment is reacted with marble has good slow speed effect, reacts corrosion rate after 10h
Only 60% or so.
The crosslinked acid fracturing fluid of the present embodiment is in 140 DEG C, shear rate 170s-1Under conditions of shear 1h after, viscosity is
91mPas illustrates that temperature tolerance is good.
Test example
By the heatproof shearing property of low corrosion green crosslinked acid fracturing fluid made from embodiment 1-5, rust inhibition, broken colloidality and sink
The production quantity of starch is according to oil and gas industry standard SY/T5107-2005《Aqueous fracturing fluid method of evaluating performance》Test
(corrosion rate and 20% hydrochloric acid compare, and determine the corrosion inhibition rate of embodiment system.20% hydrochloric acid is to the corrosion rate of steel disc
1244.5g/(m2﹒ h)), test result is as shown in table 1：
Table 1
As can be seen from Table 1, the high temperature resistant endurance of cutting energy of the low corrosion green crosslinked acid fracturing fluid in above embodiments
It is excellent, in 120 DEG C, 170s-1Under conditions of shear 1h after viscosity in 95mPas or so；React generate contents of precipitate compared with
It is low, it is 30mg/L or so；Break glue technology using capsule, break colloidality can it is good, under the conditions of 30 DEG C break adhesiveness 10mPas with
Under；Corrosion rate is lower, and corrosion inhibition rate is 97% or more.
Claims (10)
1. a kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Remaining is water, and the sum of each component mass percent is absolutely.
2. low corrosion green crosslinked acid fracturing fluid according to claim 1, which is characterized in that the organic acid is lactic acid
It is in molar ratio with gluconic acid (1-2):The mixed acid of the ratio mixing of (1-2).
3. low corrosion green crosslinked acid fracturing fluid according to claim 1, which is characterized in that the polymer thickening agent
For partially hydrolyzed polyacrylamide (PHPA) class thickening agent；Preferably, the polymer thickening agent is by acrylamide (AM) and 2- third
Acrylamide base -2- methyl-propanesulfonic acid sodium (AMPS) is 2.0~3.0 in molar ratio:1 ratio is copolymerized, polymer thickening agent
Molecular weight be 600~10,000,000.
4. low corrosion green crosslinked acid fracturing fluid according to claim 1, which is characterized in that the organic zirconium crosslinker
It is 3~4h of water-bath at a temperature of 50~55 DEG C after dissolving the water of zirconium oxychloride, isopropanol meltage, during which intermittently
Property stirring, add lactic acid and xylitol reaction 10-20min after be made.
5. low corrosion green crosslinked acid fracturing fluid according to claim 4, which is characterized in that zirconium oxychloride, water, isopropyl
Alcohol, lactic acid and xylitol mass ratio are (0.8-1.2)：(1-1.4)：(2-2.8)：(1-1.4)：(0.0-0.03)；Preferably
, zirconium oxychloride, water, isopropanol, lactic acid and xylitol mass ratio are 1:1.25:2.5:1.25:0.02.
6. low corrosion green crosslinked acid fracturing fluid according to claim 1, which is characterized in that the gel breaker is by mistake
Capsule breaker made of potassium sulfate.
7. a kind of low corrosion green crosslinked acid fracturing fluid, material quality percentage are as follows：
Remaining is water, and the sum of each component mass percent is absolutely.
8. the preparation method of low corrosion green crosslinked acid fracturing fluid described in claim 1, steps are as follows：
(1) in proportion, the lactic acid in organic acid is first added into water, stirs evenly, is then added in organic acid while stirring
Gluconic acid stirs evenly, and obtains mixed liquor；
(2) polymer thickening agent is added in the mixed liquor of step (1), stirring is to being completely dissolved, after standing 20-28h, by than
Example is added crosslinking agent and gel breaker, stirs evenly, and obtains the low corrosion green crosslinked acid fracturing fluid.
9. preparation method according to claim 8, which is characterized in that stirring after polymer thickening agent is added in step (2)
Mixing revolving speed is 400-500r/min, and gel breaker is added after crushing, and the speed of agitator after crosslinking agent and gel breaker is added is 600-
700r/min is stirred evenly and is placed in 90 DEG C of baking ovens dry 4h.
10. a kind of application of low corrosion green crosslinked acid fracturing fluid, in carbonate formation Depth Acid Fracturing technique.
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| CN111205847A (en) * | 2020-01-18 | 2020-05-29 | 海兴县新源化工有限公司 | Oil well fracturing cross-linking agent, preparation device and preparation method thereof |
| CN112375558A (en) * | 2020-11-04 | 2021-02-19 | 中国石油集团渤海钻探工程有限公司 | Working fluid system for pickling sandstone geothermal well |
| CN114437705A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Organic crosslinking acid and organic aluminum zirconium crosslinking agent for acid fracturing and preparation method thereof |
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