CN113046050A - Efficient slow-speed acidizing working fluid and preparation method thereof - Google Patents
Efficient slow-speed acidizing working fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-efficiency slow-speed acidizing working fluid and a preparation method thereof, wherein each 100 parts of the working fluid comprises the following components in parts by weight: 10 to 20 parts of ammonium salt, 5 to 20 parts of organic phosphonic acid, 5 to 20 parts of hydrochloric acid, 1 to 6 parts of corrosion inhibitor, 0.5 to 2 parts of clay stabilizer, 0.5 to 2 parts of iron ion stabilizer and the balance of water; the preparation method of the high-efficiency slow-acidification working solution comprises the steps of adding water into ammonium salt at normal temperature and normal pressure, and stirring and dissolving to obtain an ammonium salt solution; adding hydrochloric acid and organic phosphonic acid into the ammonium salt solution, and stirring and mixing uniformly to obtain a retarded acid solution; sequentially adding a corrosion inhibitor, a clay stabilizer and an iron ion stabilizer into the retarded acid solution, and uniformly stirring and mixing to obtain a finished product; the efficient slow-speed acidizing working fluid has a good corrosion effect on stratum rocks and can improve the permeability of a rock core; the oil-gas reservoir plugging agent has good retardance, can act on stratum rocks for a longer time, realizes deep plugging removal, and is beneficial to yield increase of oil-gas reservoirs.
Description
Technical Field
The invention relates to the technical field of working fluid system formulas in the processes of oil and gas exploitation acidification and acid fracturing yield increase measures, in particular to a high-efficiency slow-speed acidification working fluid and a preparation method thereof.
Background
In the process of exploiting petroleum and natural gas, in order to obtain higher oil and gas yield, usually adopt the method of acidizing and acid fracturing treatment stratum, said method is to inject the acid liquor into the wellbore through the ground high-pressure pump truck, utilize the chemical reaction of acid and mineral, remove the bottom hole pollution of producing well, water injection well, resume stratum permeability; or the acid liquor is used for corroding the stratum rock cement, so that the stratum permeability is improved, and the flow conductivity of pores and cracks is increased, so that the yield of the oil and gas well is increased, the injection of the water injection well is increased, and the purpose of increasing the yield of petroleum and natural gas is achieved.
At present, the conventional earth acid acidizing working fluid used for increasing the yield of oil and gas wells is used for acidizing sandstone reservoirs, and because the reaction speed of acid and rock is high and the action distance of acid is short, the aim of deep acidizing cannot be achieved only by eliminating the blockage of near-well stratums. In addition, as exploration and development are gradually deepened into deep wells and ultra-deep wells, more and more oil and gas wells have the characteristics of high temperature, high pressure and high fracture pressure, and the conventional acid acidizing operation seriously corrodes pipe columns and equipment. Furthermore, a large amount of the dissolved iron ions enter the formation and can potentially damage the formation. Therefore, unconventional acid fluids with deep penetration and low corrosiveness must be used for deep acidizing of the stratum to achieve the purpose of high-efficiency production increase.
Disclosure of Invention
The invention aims to provide a high-efficiency slow-speed acidizing working fluid and a preparation method thereof, and aims to solve the technical problem of preparing an unconventional acid fluid with deep penetration capacity and weak corrosivity.
In order to achieve the purpose, the specific technical scheme of the high-efficiency slow-speed acidizing working fluid and the preparation method thereof is as follows:
the efficient slow-speed acidizing working fluid comprises the following components in parts by mass per 100 parts of the working fluid: 10 to 20 parts of ammonium salt, 5 to 20 parts of organic phosphonic acid, 5 to 20 parts of hydrochloric acid, 1 to 6 parts of corrosion inhibitor, 0.5 to 2 parts of clay stabilizer, 0.5 to 2 parts of iron ion stabilizer and the balance of water.
In the high-efficiency retarded acidification working solution, the organic phosphonic acid is one or a combination of two of hydroxyethylidene diphosphonic acid and dihexyltriamine pentamethylene phosphonic acid; the ammonium salt is one or the combination of two of ammonium fluoride and ammonium bifluoride; the clay stabilizer is one or the combination of any two of ammonium chloride, potassium chloride, 2, 3-epoxypropyltrimethylammonium chloride and gamma-aminopropyltriethoxysilane; the iron ion stabilizer is one or the combination of any two of citric acid, ethylenediamine tetraacetic acid, oxalic acid and glacial acetic acid; the corrosion inhibitor is one or a combination of more of quaternary ammonium salt, Mannich base, quinoline and imidazole compounds; the water is any one of tap water or deionized water.
The preparation method of the efficient slow-speed acidizing working fluid comprises the following steps:
firstly, adding water into ammonium salt at normal temperature and normal pressure, and stirring and dissolving to obtain an ammonium salt solution;
secondly, sequentially adding hydrochloric acid and organic phosphonic acid into the ammonium salt solution obtained in the first step at normal temperature and normal pressure, and uniformly stirring and mixing to obtain a retarded acid solution;
and thirdly, sequentially adding a corrosion inhibitor, a clay stabilizer and an iron ion stabilizer into the retarded acid solution obtained in the second step at normal temperature and normal pressure, and uniformly stirring and mixing to obtain a finished product.
The preparation method of the high-efficiency slow-acidification working solution comprises the following components in parts by mass per 100 parts of the working solution: 10 to 20 parts of ammonium salt, 5 to 20 parts of organic phosphonic acid, 5 to 20 parts of hydrochloric acid, 1 to 6 parts of corrosion inhibitor, 0.5 to 2 parts of clay stabilizer, 0.5 to 2 parts of iron ion stabilizer and the balance of water.
In the preparation method of the high-efficiency retarded acidification working solution, the organic phosphonic acid is one or a combination of two of hydroxyethylidene diphosphonic acid and dihexyltriamine pentamethylene phosphonic acid; the ammonium salt is one or the combination of two of ammonium fluoride and ammonium bifluoride; the clay stabilizer is one or the combination of any two of ammonium chloride, potassium chloride, 2, 3-epoxypropyltrimethylammonium chloride and gamma-aminopropyltriethoxysilane; the iron ion stabilizer is one or the combination of any two of citric acid, ethylenediamine tetraacetic acid, oxalic acid and glacial acetic acid; the corrosion inhibitor is one or a combination of more of self-developed quaternary ammonium salt, Mannich base, quinoline and imidazole compounds; the water is any one of tap water or deionized water.
The efficient slow-speed acidizing working fluid and the preparation method thereof have the following advantages: the preparation method of the efficient slow-speed acidizing working fluid is simple, raw materials are easy to obtain, and the purposes of removing blockage in deep stratum and increasing yield efficiently can be achieved. The efficient retarded acidizing working fluid has good corrosion resistance and retarding property, can act on stratum rocks for a longer time, prolongs the acid rock reaction time, and achieves the purpose of deep blockage removal; the core permeability can be obviously improved, and the purpose of high-efficiency production increase can be achieved; the corrosion inhibitor has low corrosion resistance to N80 type metal pipes and equipment, and shows good corrosion inhibition effect; the method also has the characteristic of easy flowback, and can effectively reduce secondary damage to the reservoir.
Drawings
FIG. 1 is a graph showing erosion rates of different types of acidizing working fluids on rock powder in example 3 of the present invention.
FIG. 2 is a graph illustrating the increase in core permeability for different types of acidizing fluids according to example 4 of the present invention.
FIG. 3 is a graph showing the corrosion rates of different types of acidified working liquids on a sample of N80 type steel in example 5 of the present invention.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the efficient retarded acidification working fluid and the preparation method thereof are further described in detail below with reference to the accompanying drawings.
Example 1:
the first preparation of efficient slow acidifying liquid.
Setting the mass of the high-efficiency slow-speed acidification working solution to be prepared as 100 parts; under the conditions of normal temperature and normal pressure, firstly, preparing an ammonium salt solution with the mass fraction of 10% by using tap water and ammonium bifluoride; sequentially adding a certain amount of hydrochloric acid, hydroxyethylidene diphosphonic acid and ammonium bifluoride into the ammonium salt solution, stirring and uniformly mixing to obtain a retarded acid solution with the mass fraction of 12% of hydrochloric acid, 15% of hydroxyethylidene diphosphonic acid and 10% of ammonium bifluoride; and then adding quantitative self-developed Mannich base corrosion inhibitors, a clay stabilizer ammonium chloride and an iron ion stabilizer ethylene diamine tetraacetic acid into the retarded acid solution, stirring and uniformly mixing to obtain a first efficient retarded acidification working solution with the mass fraction of 12% of hydrochloric acid, 15% of hydroxyethylidene diphosphonic acid, 10% of ammonium bifluoride, 2% of Mannich base corrosion inhibitors, 1% of clay stabilizer ammonium chloride and 1% of iron ion stabilizer ethylene diamine tetraacetic acid.
Example 2:
and preparing a second efficient slow-speed acidizing working solution.
Setting the mass fraction of the acidizing working fluid to be prepared as 100; under the conditions of normal temperature and normal pressure, firstly, preparing an ammonium salt solution with the mass fraction of 15% by using tap water and ammonium fluoride; then, adding hydrochloric acid, hydroxyethylidene diphosphonic acid and dihexyltriamine pentamethylene phosphonic acid (mass fraction is 1:1) into the ammonium salt solution in sequence, stirring and uniformly mixing to obtain a retarded acid solution with the mass fraction of 12% of hydrochloric acid, the mass fraction of 15% of hydroxyethylidene diphosphonic acid and dihexyltriamine pentamethylene phosphonic acid and the mass fraction of 15% of ammonium fluoride; and adding a certain amount of self-developed quaternary ammonium salt, an imidazole corrosion inhibitor, a clay stabilizer potassium chloride and an iron ion stabilizer citric acid into the retarded acid solution, stirring and uniformly mixing to obtain a second efficient retarded acidification working solution, wherein the mass fraction of the hydrochloric acid is 12%, the mass fraction of the hydroxyethylidene diphosphonic acid is 15%, the mass fraction of the ammonium fluoride is 15%, the mass fraction of the quaternary ammonium salt and the imidazole corrosion inhibitor is 2.5%, the mass fraction of the clay stabilizer potassium chloride is 0.5%, and the mass fraction of the iron ion stabilizer citric acid is 0.5%.
Example 3:
and (3) carrying out an experiment on the corrosion rate of the high-efficiency slow-speed acidizing working solution on the rock powder.
Drying the rock powder at 80 deg.C for 4h, and sealing in a drying bottle. And taking out the dried rock powder at room temperature, and weighing the rock powder, wherein the mass of each part is 5.0000 g. Putting rock powder and different acid solutions into a wide-mouth bottle according to the using amount of 10ml of 1g of rock powder acid solution, oscillating to enable the acid solution to be fully contacted with the rock powder, standing, filtering by using filter paper after reacting for different time, drying residues at 80 ℃ for 6 hours, and weighing the mass of the filter paper and the residues. The corrosion rate of the rock powder was calculated from the mass of the rock powder before and after the reaction by using the formula (1), and the calculation results are shown in table 1. All waste liquids are poured into the waste liquid recycling bin and are treated in a unified mode in the experiment.
Wherein the content of the first and second substances,m1is the initial mass of rock dust, g; m is2The mass of the rock dust which is not corroded after filtration, g.
TABLE 1 dissolution rates of different acidizing fluids on sandstone powders
As can be seen from table 1, compared with the conventional earth acid acidizing working fluid, the two high-efficiency slow acidizing working fluids provided by the embodiment of the invention have slightly lower erosion rates to rock powder; after two hours of reaction, the corrosion rate of the conventional earth acid acidizing working fluid to rock powder is almost not increased along with the prolonging of the reaction time any more; the erosion rate of the high-efficiency retarded acidizing working fluid on rock powder is continuously increased along with the prolonging of the reaction time, which shows that the high-efficiency retarded acidizing working fluid provided by the embodiment of the invention can act on stratum rocks for a longer time, and the defects that the conventional earth acid acidizing working fluid reacts with the stratum rocks too fast to cause short acid liquid acting distance and the deep blockage removal cannot be realized are effectively avoided.
As shown in fig. 1, the erosion rate graphs of rock powder for two types of high-efficiency retarded acidizing working fluids in this embodiment. From the graph, it can be seen that the erosion rate of the high-efficiency retarded acidizing working fluid provided by the embodiment of the invention on rock powder is obviously increased along with the prolonging of the reaction time, which shows that the high-efficiency retarded acidizing working fluid provided by the embodiment of the invention can continuously release H along with the continuous proceeding of the reaction+And stratum rocks are continuously and effectively dissolved, and deep blockage removal is realized.
Example 4:
and (3) testing the influence of the high-efficiency slow-speed acidizing working fluid on the permeability of the rock core.
Putting the rock core into a rock core holder, setting the initial value of confining pressure to be 2MPa, setting the injection flow rate q of working fluid to be 1ml/min, firstly injecting 3% KCl as a front liquid, measuring the real-time permeability K of the rock core to a certain liquid volume when liquid seeps from a downstream outlet, and calculating the average value K of the permeability of the rock core in the time periodi. Stopping the injection of the pre-solution, opening the acid solution control valve, and acidifyingAnd injecting working liquid into the rock core, and measuring the real-time permeability K of the rock core until the upstream pressure is reduced constantly when liquid seeps out from the downstream outlet. Closing the acid liquid control valve, injecting 3% KCl as a post liquid again, measuring the real-time permeability K of the rock core until a certain liquid volume is injected when liquid seeps from a downstream outlet, and calculating the average value K of the rock core permeability in the time periodf. The change in core permeability during acidizing was calculated and the results are shown in table 2.
TABLE 2 influence of different acidizing fluids on sandstone core permeability
As can be seen from table 2, the permeability of the core increased by 13.57 times under the novel high-efficiency retarded acidizing working fluid of example 1; under the novel efficient slow-speed acidizing working fluid of the embodiment 2, the permeability of the rock core is increased by 13.64 times, and the increase rate of the permeability of the rock core is far greater than that of the conventional earth acid acidizing working fluid. The novel efficient slow-speed acidizing working fluid provided by the embodiment of the invention can effectively increase the permeability of a reservoir and realize efficient production increase.
As shown in fig. 2, the increase multiple ratio of the permeability of the core by the two types of high-efficiency retarded acidizing working fluids in this embodiment is shown. As can be seen from the figure, the increase ratios of the two high-efficiency retarded acidizing working fluids provided by the embodiment of the present invention to the core permeability are substantially the same, which indicates that the high-efficiency retarded acidizing working fluids prepared by the preparation method provided by the embodiment of the present invention have similar performance, that is, the preparation method is effective and feasible, and various changes or equivalent replacements can be performed according to the preparation method to prepare more different types of high-efficiency retarded acidizing working fluids.
Example 5:
and (3) carrying out corrosion rate experiment on the N80 section steel sample by using the high-efficiency slow-speed acidizing working solution.
The steps of the embodiment are carried out according to the oil and gas industry standard of the people's republic of China (SY/T5405-1996), and the specific process is as follows:
taking out the N80 type standard corrosion test piece, measuring the size of the standard corrosion test piece by using a vernier caliper, and recording and calculating the surface area;
pretreating an N80 test piece (degreasing with acetone, degreasing with ethanol, and naturally air drying), weighing with an electronic balance (4 positions after decimal point is achieved), and recording the initial mass m1；
The consumption of acid solution is 20cm per square centimeter of test piece surface area3Sequentially pouring different types of acidizing working solutions into a plastic beaker;
suspending the test piece in a slow acidification working solution to ensure that the test piece is completely soaked in the liquid and is not in contact with the bottom and the wall of the beaker, and covering the surface of the beaker with a preservative film;
placing the beaker in a water bath kettle with the constant temperature of 90 ℃; recording the reaction starting time, taking out the test piece after 4 hours of reaction, immediately washing the test piece with tap water, then brushing the test piece with a soft brush, finally cleaning the test piece with absolute ethyl alcohol, wiping the surface of the test piece with filter paper, weighing the test piece with an electronic balance (accurate to 4 decimal places), and recording the mass m after the reaction2(ii) a And (6) taking a picture.
The corrosion rate v was calculated using the following formula, and the results are shown in table 3.
Wherein v isiCorrosion Rate of the monolithic sample, g/(m)2H); t: reaction time, h; m is1: mass of the sample before corrosion, g; m is2: mass g of the sample after corrosion; a: surface area of sample, mm2。
TABLE 3 atmospheric static etch rates (90 ℃ C.) for standard etch specimens of type N80 in different acidified working fluids
As can be seen from Table 3, the corrosion rate of the novel efficient retarded acidification working solution provided by the embodiment of the invention on the N80 test piece is lower than that of the conventional earth acid acidification working solution on the N80 test piece after the corrosion inhibitor is addedCorrosion rate and is much less than the first order index value (3 to 4 g.m) for 12% HCl + 3% HF in the SY/T5405-1996 industry Standard-2·h-1). The N80 type standard corrosion test piece soaked by the novel efficient retarded acidification working solution provided by the embodiment of the invention has the advantages of complete surface, very low overall corrosion degree and no obvious visible local corrosion pit, so that the novel efficient retarded acidification working solution provided by the embodiment of the invention has small damage to a pipe and shows low corrosivity, and the safety of a downhole pipe column and construction equipment is guaranteed.
As shown in FIG. 3, the corrosion rates of two types of high-efficiency retarded acidification working fluids on a sample of N80 type steel in the embodiment of the invention are shown schematically. As can be seen from the figure, the corrosion rate of the high-efficiency slow-speed acidizing working fluid provided by the embodiment of the invention on the N80 section steel sample is only 1/2 of that of the conventional earth acid acidizing working fluid, and the safety of construction operation can be further ensured.
In summary, the features of the novel efficient retarded acidification working fluid and the preparation method thereof provided by the invention can be combined with each other in the above embodiments without conflict.
The content that is not described in this embodiment is the prior art, and therefore, the description thereof is omitted.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. The efficient slow-speed acidizing working fluid is characterized in that each 100 parts of the working fluid comprises the following components in parts by mass: 10 to 20 parts of ammonium salt, 5 to 20 parts of organic phosphonic acid, 5 to 20 parts of hydrochloric acid, 1 to 6 parts of corrosion inhibitor, 0.5 to 2 parts of clay stabilizer, 0.5 to 2 parts of iron ion stabilizer and the balance of water.
2. The efficient retarded acidizing fluid of claim 1 wherein said organic phosphonic acid is one or a combination of two of hydroxyethylidene diphosphonic acid, dihexyltriamine pentamethylene phosphonic acid;
the ammonium salt is one or the combination of two of ammonium fluoride and ammonium bifluoride;
the clay stabilizer is one or the combination of any two of ammonium chloride, potassium chloride, 2, 3-epoxypropyltrimethylammonium chloride and gamma-aminopropyltriethoxysilane;
the iron ion stabilizer is one or the combination of any two of citric acid, ethylenediamine tetraacetic acid, oxalic acid and glacial acetic acid;
the corrosion inhibitor is one or a combination of more of quaternary ammonium salt, Mannich base, quinoline and imidazole compounds;
the water is any one of tap water or deionized water.
3. The preparation method of the high-efficiency slow-speed acidizing working fluid as claimed in claim 1, which comprises the following steps:
firstly, adding water into ammonium salt at normal temperature and normal pressure, and stirring and dissolving to obtain an ammonium salt solution;
secondly, sequentially adding hydrochloric acid and organic phosphonic acid into the ammonium salt solution obtained in the first step at normal temperature and normal pressure, and uniformly stirring and mixing to obtain a retarded acid solution;
and thirdly, sequentially adding a corrosion inhibitor, a clay stabilizer and an iron ion stabilizer into the retarded acid solution obtained in the second step at normal temperature and normal pressure, and uniformly stirring and mixing to obtain a finished product.
4. The preparation method of the efficient slow-speed acidizing working fluid according to the claim 3, wherein each 100 parts of the working fluid comprises the following components in parts by mass: 10 to 20 parts of ammonium salt, 5 to 20 parts of organic phosphonic acid, 5 to 20 parts of hydrochloric acid, 1 to 6 parts of corrosion inhibitor, 0.5 to 2 parts of clay stabilizer, 0.5 to 2 parts of iron ion stabilizer and the balance of water.
5. The method for preparing the working fluid with high efficiency and slow acidification according to claim 3, wherein the organic phosphonic acid is one or a combination of two of hydroxyethylidene diphosphonic acid and dihexyltriamine pentamethylene phosphonic acid;
the ammonium salt is one or the combination of two of ammonium fluoride and ammonium bifluoride;
the clay stabilizer is one or the combination of any two of ammonium chloride, potassium chloride, 2, 3-epoxypropyltrimethylammonium chloride and gamma-aminopropyltriethoxysilane;
the iron ion stabilizer is one or the combination of any two of citric acid, ethylenediamine tetraacetic acid, oxalic acid and glacial acetic acid;
the corrosion inhibitor is one or a combination of more of quaternary ammonium salt, Mannich base, quinoline and imidazole compounds;
the water is any one of tap water or deionized water.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074050A (en) * | 2011-10-26 | 2013-05-01 | 中国石油化工股份有限公司 | Anti-scaling multi-hydrogen retarded acid for highly argillaceous sandstone reservoir |
| RU2616949C1 (en) * | 2016-02-29 | 2017-04-18 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Acid composition for treatment of low permeable high temperature formations with high clay and carbonates content |
| CN108219763A (en) * | 2018-01-20 | 2018-06-29 | 中国石油集团渤海钻探工程有限公司 | A kind of acidizing sandstone oil reservoir slow type MH acid system and its construction technology |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103074050A (en) * | 2011-10-26 | 2013-05-01 | 中国石油化工股份有限公司 | Anti-scaling multi-hydrogen retarded acid for highly argillaceous sandstone reservoir |
| RU2616949C1 (en) * | 2016-02-29 | 2017-04-18 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Acid composition for treatment of low permeable high temperature formations with high clay and carbonates content |
| CN108219763A (en) * | 2018-01-20 | 2018-06-29 | 中国石油集团渤海钻探工程有限公司 | A kind of acidizing sandstone oil reservoir slow type MH acid system and its construction technology |
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Application publication date: 20210629 |