CN113528115A - Low-temperature guar gel breaker for oil-gas well fracturing, preparation method and application - Google Patents
Low-temperature guar gel breaker for oil-gas well fracturing, preparation method and application Download PDFInfo
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Abstract
The invention belongs to the technical field of fracturing fluid chemicals in the process of oil and gas field exploitation, and discloses a low-temperature guar gel breaker for oil and gas well fracturing, a preparation method and application thereof, wherein the low-temperature guar gel breaker for oil and gas well fracturing consists of 58% of beta-D-glycuronidase, 0.1% -1.0% of a composite initiator, 12% -23% of hydroxyalkyl chitosan, 5% -12% of tetramethyl ammonium cage-shaped polysilsesquioxane, 10% -15% of polyethylene glycol and 5% -8% of water in percentage by mass. The preparation method comprises the following steps: adding beta-D-glycoside dew polysaccharide enzyme liquid, hydroxyalkyl chitosan and water into a reaction kettle and mixing; adding a composite initiator, stirring, and adding tetramethyl ammonium cage-shaped polysilsesquioxane; adding polyethylene glycol, stirring, and cooling to room temperature to obtain the low-temperature guar gel breaker for oil-gas well fracturing. The invention has the advantages of wide application range, small damage to stratum, high flowback rate and realization of rapid gel breaking.
Description
Technical Field
The invention belongs to the technical field of fracturing fluid chemicals in the process of exploitation of oil and gas fields, and particularly relates to a low-temperature guar gel breaker for oil and gas well fracturing, a preparation method and application.
Background
Fracturing is the most effective means for increasing the yield and injection of oil-water wells in the current oil-gas field development process. Wherein, the success or failure of the fracturing fluid directly influences the success or failure of the fracturing. The traditional fracturing fluid generally adopts potassium persulfate, ammonium persulfate, capsule gel breakers, acidic gel breakers and other gel breakers, and has the following defects: the gel breaker system reacts with the fracturing string column in the fracturing construction process, iron ions are easy to form indissolvable precipitates in the stratum to block the pores of the matrix while the string column is corroded, and in addition, part of the gel breaker system also easily reacts with clay minerals, crude oil and the like in the matrix of the stratumAn emulsion which is extremely difficult to treat is generated, and the fracturing fluid system is difficult to treat after flowback, so that the treatment cost of the fracturing fluid is greatly increased; the oxidation gel breaking system has certain randomness during gel breaking, polymer macromolecules can not be completely degraded, and the polymer macromolecules are larger than 2.0 multiplied by 10 according to statistics6About 20% of the fracturing fluid is not degraded after being broken by using the oxidation gel breaker; meanwhile, the degree of mineralization of the fracturing fluid can be increased by adding the conventional gel breaker, the pipe column can be corroded in the fracturing process, and the electric field of the crude oil electric dehydrator can be failed and the dehydration fails due to the fact that the flowback liquid enters the system after fracturing.
Thus, new types of breakers have been studied. The biological enzyme gel breaking is an important research direction, can realize the purposes of high-efficiency gel breaking and no corrosion to a tubular column and underground equipment, does not need to change the existing fracturing process, and has low operation cost and high input-output ratio.
Through the above analysis, the problems and defects of the prior art are as follows: the purposes of high-efficiency gel breaking and no corrosion to a pipe column and underground equipment are achieved, the existing fracturing process is not required to be changed, the operation cost is low, and the input-output ratio is high.
The difficulty in solving the above problems and defects is: the guanidine gum fracturing liquid system is difficult to break gum at the temperature below 30 ℃ through the existing normal-temperature gel breaking system, adsorption and retention damage is caused to a modified stratum, the biological enzyme gel breaking activation performance is high, and normal-temperature storage and transportation are the technical key which needs to be broken through urgently at present.
The significance of solving the problems and the defects is as follows: the application of the guanidine gum fracturing fluid in a low-temperature well is greatly promoted, the storage and transportation of a low-temperature gel breaking technology under normal temperature and normal pressure are further broken through, and the problem that the vegetable gum is difficult to break under low-temperature and low-pressure conditions is solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a low-temperature guar gel breaker for oil-gas well fracturing, a preparation method and application thereof.
The low-temperature guar gum breaker for oil-gas well fracturing is prepared from 58% of beta-D-glycuronide 58%, 0.1-1.0% of a composite initiator (TDS), 12-23% of hydroxyalkyl chitosan, 5-12% of tetramethyl ammonium cage polysilsesquioxane, 10-15% of polyethylene glycol and 5-8% of water in percentage by mass.
The invention also aims to provide a preparation method of the low-temperature guar gel breaker for oil and gas well fracturing, which comprises the following steps:
firstly, adding beta-D-glycoside dew polysaccharide enzyme liquid, hydroxyalkyl chitosan and water into a reaction kettle and mixing;
secondly, adding a composite initiator, stirring, and adding tetramethyl ammonium polyhedral oligomeric silsesquioxane;
and step three, adding polyethylene glycol, stirring, and cooling to room temperature to obtain the low-temperature guar gel breaker for oil-gas well fracturing.
And further, adding the composite initiator in the second step, and stirring for 20-30 min.
Further, the second step was to add tetramethylammonium cage polysilsesquioxane and the temperature was maintained at 15 ℃.
And further, polyethylene glycol is added in the third step, and stirring is carried out for 1.5 h.
Further, the third step is carried out at room temperature of 15 ℃ or below.
The invention also aims to provide a fracturing fluid which comprises the low-temperature guar gel breaker for oil and gas well fracturing.
The invention also aims to provide a method for increasing the yield and the injection of the oil-water well, which uses the fracturing fluid.
By combining all the technical schemes, the invention has the advantages and positive effects that: the invention mainly relates to a biological enzyme gel breaker which is mainly beta-D-glycoside dewanase, is a specific hydrolase and is specifically used for beta-1, 4-bond glycoside bonds of polysaccharide polymers. The biological enzyme gel breaker has the advantages of low temperature (20-60 ℃), pH (3-11), specificity, high efficiency and wide application range, and the biological enzyme gel breaker has the advantages of wide application range, small damage to stratum, high flowback rate, no pollution to environment and the like, and is widely applied in practice. Aiming at the fact that the low-temperature gel breaker of the system has low temperature (20-60 ℃), pH (3-11), specificity, high efficiency and wide application range, and the low-temperature gel breaker has the advantages of wide application range, small damage to stratum and high flowback rate, the preparation method and the evaluation method of the gel breaker are provided, damage of fracturing fluid to oil and gas wells can be effectively and quickly removed, and an excellent product for quickly breaking gel is realized.
The low-temperature fracturing fluid system comprises the following components: 0.30 percent of guanidine gum, 2 percent of KCl, 0.1 percent of bactericide, 0.5 percent of clay stabilizer, 0.7 percent of cleanup additive, 0.1 percent of waterproof locking agent, 0.5 percent of foaming agent and 0.1 percent of nano cleanup additive. A crosslinking agent: 0.3% guar gum + others. A gel breaker: a biological enzyme gel breaker. The gel breaker of the fracturing fluid system of the low-temperature gas well is biological enzyme, the main component of the gel breaker is beta-D-glycoside dewanase, and the gel breaker is a specific hydrolase and is specifically used for beta-1, 4-bond glycosidic bond of polysaccharide polymer. The beta-glycoside mannase is an incision enzyme, greatly reduces the viscosity and the molecular weight of guar gum through the incision action, and directly acts on glycosidic bonds to mainly generate di-hexa-oligosaccharide with little monosaccharide. The fracturing fluid can degrade thickening agents containing mannan, such as guar gum, modified guar gum, xanthan gum, konjac gum and the like, and can be returned to the ground by reducing the viscosity of the fracturing fluid, so that the damage of the fracturing fluid to the stratum and the environmental pollution are reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
FIG. 1 shows a low-temperature guar gel breaker for oil and gas well fracturing, a preparation method and application thereof
FIG. 2 is a schematic diagram showing the effect of temperature on gel breaking performance of biological enzymes according to an embodiment of the present invention.
FIG. 3 is a graph showing the effect of pH on the activity of biological enzymes according to an embodiment of the present invention.
Fig. 4 is a schematic diagram of a fluid loss curve at 80 c provided by an embodiment of the present invention.
Fig. 5 is a schematic diagram of the temperature resistance and shear resistance of the fracturing fluid system provided by the embodiment of the invention at 60 ℃.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a low-temperature guar gel breaker for oil-gas well fracturing, a preparation method and application thereof, and the invention is described in detail below with reference to the accompanying drawings.
The low-temperature guar gel breaker for oil-gas well fracturing comprises, by mass, 58% of beta-D-glycoside mannase, 0.1% -1.0% of a composite initiator, 12% -23% of hydroxyalkyl chitosan, 5% -12% of tetramethyl ammonium cage-shaped polysilsesquioxane, 10% -15% of polyethylene glycol and 5% -8% of water.
As shown in figure 1, the preparation method of the low-temperature guar gel breaker for oil and gas well fracturing provided by the invention comprises the following steps:
s101: adding beta-D-glycoside dew polysaccharide enzyme liquid, hydroxyalkyl chitosan and water into a reaction kettle and mixing;
s102: adding a composite initiator, stirring for 20-30min, adding tetramethylammonium polyhedral oligomeric silsesquioxane, and keeping the temperature at 15 ℃;
s103: adding polyethylene glycol, stirring for 1.5h, and cooling to room temperature (storing below 15 deg.C) to obtain low temperature guar gel breaker for oil gas well fracturing.
The preparation method of the low-temperature guar gel breaker for oil and gas well fracturing provided by the invention can be implemented by other steps by persons skilled in the art, and the preparation method of the low-temperature guar gel breaker for oil and gas well fracturing provided by the invention shown in fig. 1 is only a specific example.
The technical solution of the present invention is further described with reference to the following examples.
Example 1
The low-temperature guar gum gel breaker for fracturing of oil and gas wells provided by the invention comprises the following components in percentage by mass: 58% of beta-D-glycoside mannase, 16% of hydroxyalkyl chitosan, 0.5% of composite initiator, 12% of polyethylene glycol, 10% of tetramethyl ammonium cage polysilsesquioxane and 3.5% of water.
The invention provides a preparation method of a low-temperature guar gel breaker for fracturing of an oil-gas well, which comprises the following steps: 0.58kg of beta-D-glycanase, 0.16kg of hydroxyalkyl chitosan, 0.005kg of composite initiator, 0.12kg of polyethylene glycol, 0.1kg of tetramethyl ammonium cage polysilsesquioxane and 0.035kg of water are stirred and reacted for 2 hours at the temperature of 15 ℃ to prepare the low-temperature biological enzyme gel breaker product.
Example 2
The low-temperature guar gum gel breaker for fracturing of oil and gas wells provided by the invention comprises the following components in percentage by mass: 55% of beta-D-glycoside mannase, 18% of hydroxyalkyl chitosan, 0.8% of composite initiator, 15% of polyethylene glycol, 6% of tetramethyl ammonium cage polysilsesquioxane and 5.2% of water.
The invention provides a preparation method of a low-temperature guar gel breaker for fracturing of an oil-gas well, which comprises the following steps: 0.55kg of beta-D-glycanase, 0.18kg of hydroxyalkyl chitosan, 0.008kg of composite initiator, 0.15kg of polyethylene glycol, 0.06kg of tetramethyl ammonium cage polysilsesquioxane and 0.052kg of water are stirred and react for 2 hours at the temperature of 15 ℃ to prepare the low-temperature biological enzyme gel breaker product.
Example 3
The low-temperature guar gum gel breaker for fracturing of oil and gas wells provided by the invention comprises the following components in percentage by mass: 60% of beta-D-glycoside mannase, 13% of hydroxyalkyl chitosan, 0.7% of composite initiator, 13% of polyethylene glycol, 9% of tetramethyl ammonium cage polysilsesquioxane and 4.3% of water.
The invention provides a preparation method of a low-temperature guar gel breaker for fracturing of an oil-gas well, which comprises the following steps: 0.6kg of beta-D-glycoside mannase, 0.13kg of hydroxyalkyl chitosan, 0.007kg of composite initiator, 0.13kg of polyethylene glycol, 0.09kg of tetramethyl ammonium cage polysilsesquioxane and 0.043kg of water are stirred and react for 2 hours at the temperature of 15 ℃ to prepare the low-temperature biological enzyme gel breaker product.
Example 4
The low-temperature guar gum gel breaker for fracturing of oil and gas wells provided by the invention comprises the following components in percentage by mass: 58% of beta-D-glycoside mannase, 12% of hydroxyalkyl chitosan, 0.6% of composite initiator, 14% of polyethylene glycol, 12% of tetramethyl ammonium cage polysilsesquioxane and 3.4% of water.
The invention provides a preparation method of a low-temperature guar gel breaker for fracturing of an oil-gas well, which comprises the following steps: 0.58kg of beta-D-glycuronide, 0.12kg of hydroxyalkyl chitosan, 0.006kg of composite initiator, 0.14kg of polyethylene glycol, 0.12kg of tetramethyl ammonium cage polysilsesquioxane and 0.034kg of water are stirred and react for 2 hours at the temperature of 15 ℃ to prepare the low-temperature biological enzyme gel breaker product.
Example 5
And (4) evaluating the enzyme activity of the biological enzyme gel breaker. The cuvette (3 equal experiments are needed), the zero adjustment is carried out by using p-nitrophenol-beta-D-galactoside, 950 mu L of p-nitrophenol-beta-D-galactoside is added, the temperature is kept for 1min at 80 ℃, 50 mu L of bio-enzyme gel breaker sample is added for fully mixing, no air bubble is generated, and the light absorption value is measured by using a 10mm cuvette under the condition that the wavelength is 405 nm. Activity (U/mL) ═ dilution factor × average absorbance per minute × assigned standard value/standard sample average absorbance per minute.
Example 6
And (4) measuring the viscosity of the gel breaking liquid by using a viscosity meter.
A certain amount of liquid to be measured is taken by a pipette and put into a viscometer, and the viscometer is vertically fixed on an iron stand to ensure that the viscometer is vertical to the ground. The liquid is sucked by the suction ear ball and rises to the 2/3 position of the ball, the suction is stopped, and the pipe orifice is blocked. The time required for the liquid to flow between the two scales was measured using a stopwatch. The measurement was repeated 3 times and the average value was obtained. The obtained time is multiplied by a coefficient to obtain the viscosity (mPas) of the solution.
Example 7
And (3) evaluating the influence of the fracturing fluid additive on the enzyme activity through an experiment.
Biological enzyme is selected as the gel breaker, and the compatibility of the enzyme and the fracturing fluid additive is ensured. The gel breaking condition of the biological enzyme under different fracturing fluid additives is shown in table 1. As can be seen from Table 1, no incompatibility exists among the clay stabilizer, the anti-swelling agent, the cleanup additive, the bactericide, the temperature stabilizer and the like for the biological enzyme, and the viscosity of the gel breaking solution is less than 5 mPas after 3 hours.
TABLE 1 gel breaking of biological enzymes with different oilfield additives
Example 8
And (3) experimental evaluation of influence factors of biological enzyme gel breaking.
(1) The effect of temperature on the activity of the biological enzymes is shown in FIG. 2. As can be seen from FIG. 2, the viscosity of the gel breaking liquid of the low-temperature enzyme gel breaker is less than 5mPa & s within the range of 20-60 ℃, and the activity of the enzyme can be influenced when the viscosity is higher or lower than the temperature range; the applicable temperature ranges of the medium-high temperature enzyme gel breaker and the high-temperature enzyme gel breaker are 60-100 ℃ and 90-120 ℃, respectively, and the low-temperature biological enzyme gel breaker has a good gel breaking effect in the well temperature range of 20-60 ℃.
(2) The effect of pH on the biological enzyme activity is shown in FIG. 3. As can be seen from FIG. 3, the optimum action condition of the enzyme is that the pH value is 6-8, and the enzyme activity is higher than 150U/mL under the condition, wherein the optimum pH value of the enzyme activity is 7.
(3) The surface tension, interfacial tension and residue content of the flowback fluid after breaking gel with the bio-enzyme are shown in table 2. As can be seen from Table 2, the fracturing fluid has lower surface tension and interface tension after being broken by 3 biological enzymes, and is easy to flow back; the content of the residue is not more than 205mg/L and is lower than the industrial standard of 500 mg/L. The gel breaker can reduce the viscous resistance of the fracturing fluid and reduce the damage of high molecular substances to the stratum.
Table 2: surface interfacial tension and residue content of fracturing fluid after biological enzyme action
The technical effects of the present invention will be described in detail with reference to experiments.
1. The quality of the biological enzyme gel breaker prepared by the method of the invention reaches the following technical indexes, and is shown in table 3.
TABLE 3 technical indices of the products
2. The invention also provides an evaluation method of the low-temperature gas well fracturing fluid system, which is characterized by measuring the compatibility, the crosslinking performance and the filtration loss performance of the low-temperature fracturing fluid, and measuring the gel breaking time (20-60 ℃), the viscosity of the gel breaking fluid, the residue content of the gel breaking fluid, the viscosity retention rate and the enzyme activity.
(1) Determination of compatibility
All additives except the thickening agent are sequentially added indoors according to the formula of the fracturing fluid system, the mixture is respectively placed for 48 hours at room temperature and the temperature of the stratum corresponding to the additive, and the observation shows that the solution is clear, no precipitate or floccule appears, and the additive of the fracturing fluid formula has good compatibility.
TABLE 4 fracturing fluid system compatibility analysis
(2) Crosslinking Properties
According to the formula of a fracturing system, the gelling condition of the fracturing fluid is tested at a cross-linking ratio of 50: 1 indoors, and the result shows that the fracturing fluid is good in cross-linking state and can be hung.
(3) Fluid loss performance
The static fluid loss performance of the fracturing fluid formula is evaluated by a GGS71 type high-temperature high-pressure fluid loss instrument indoors, the experimental temperature is 80 ℃ and 80 ℃, and the experimental result is shown in figure 4.
TABLE 5 fluid loss Performance of fracturing fluid systems at different temperatures
| Temperature of | Technical index | The result of the detection |
| Fluid loss coefficient, m/min1/2 | ≤1.0×10-3 | 0.09×10-4 |
| Fluid loss rate,. times.10-4 m3/m2 | 1.5×10-4 | 0.015×10-4 |
| Initial filtration loss m/min | 5.0×10-2 | 0.63×10-3 |
(4) Temperature and shear resistance
The temperature resistance and shear resistance of the fracturing fluid formula at 80 ℃ is evaluated indoors by adopting a Mars40 rheometer of the German HAKE company, and the experimental result is shown in figure 5.
TABLE 6 temperature and shear resistance test data
| Temperature/. degree.C | 41.04 | 60.01 | 59.95 | 59.95 |
| Time/min | 4.188 | 16.01 | 80.15 | 120 |
| viscosity/mPas | 361.5 | 191.7 | 215.0 | 217.3 |
The cross ratio is 50: 1, the temperature resistance and shear resistance curve at 80 ℃ is realized, and the tail is stuck to more than 200mPa & s after 120 minutes; the system meets the transformation requirement of a reservoir stratum at 35-65 ℃.
(5) And (5) measuring gel breaking time.
Taking two closed containers, respectively measuring 100mL of fracturing fluid jelly therein, respectively placing the containers in a constant-temperature water bath kettle at a constant temperature of 20-60 ℃, respectively measuring 0.5mL of biological enzyme diluent by using a pipette, adding the biological enzyme diluent into the containers, and uniformly mixing the containers to ensure that the fracturing fluid breaks gel under a constant-temperature gradient.
And observing the apparent viscosity change of the fracturing fluid at regular intervals. And if the apparent viscosity is lower by visual inspection, measuring the viscosity of the gel breaking liquid at different time by using a capillary viscometer. And drawing a curve by taking the time as an abscissa and the viscosity of the gel breaking solution as an ordinate, reading the constant temperature time when the apparent viscosity of the gel breaking solution is 5.0mPa & s from the curve, recording the constant temperature time as gel breaking time, and respectively measuring the gel breaking time of the gel at the temperature of between 20 and 60 ℃.
(6) Viscosity measurement of gel breaker
The measurement of the residue content of the gel breaking solution was carried out in accordance with the specification of 6.13 in SY/T5107-2005.
(7) Determination of residue content in gel breaking liquid
The measurement of the residue content of the gel breaking solution was carried out in accordance with the specification of 6.14 in SY/T5107-2005.
(8) Measurement of viscosity Retention
The measurement of the viscosity retention of the fracturing fluid was carried out according to the specification of 10.2 in SY/T6380-2008. The test temperature was 50 ℃.
(9) Enzyme activity assay
Taking 4 tubes with 10mL scale, one tube as blank control, adding 0.05mL enzyme solution to the other 3 tubes, adding 1.45mL 0.5% locust bean gum solution to each of the 4 tubes, and reacting at 50 deg.C for 23min (preheating for the first 3 min). Taking out, rapidly cooling, adding 2mL of dinitro salicylic acid (dinitro salicylic acid) reagent, adding 0.05mL of enzyme solution into a blank tube, and boiling in boiling water for 5 min. After cooling, distilled water was added to the solution to a constant volume of 10mL, and the mixture was thoroughly mixed, and absorbance was measured at 540 nm. And (4) calculating the enzyme activity.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The low-temperature guar gum breaker for oil and gas well fracturing is characterized by comprising, by mass, 58% of beta-D-glycuronide 58, 0.1-1.0% of a composite initiator, 12-23% of hydroxyalkyl chitosan, 5-12% of tetramethyl ammonium cage polysilsesquioxane, 10-15% of polyethylene glycol and 5-8% of water.
2. The preparation method of the low-temperature guar gel breaker for oil and gas well fracturing as claimed in claim 1, wherein the preparation method of the low-temperature guar gel breaker for oil and gas well fracturing comprises the following steps:
firstly, adding beta-D-glycoside dew polysaccharide enzyme liquid, hydroxyalkyl chitosan and water into a reaction kettle and mixing;
secondly, adding a composite initiator, stirring, and adding tetramethyl ammonium polyhedral oligomeric silsesquioxane;
and step three, adding polyethylene glycol, stirring, and cooling to room temperature to obtain the low-temperature guar gel breaker for oil-gas well fracturing.
3. The method for preparing the low-temperature guar gel breaker for oil and gas well fracturing as claimed in claim 2, wherein the compound initiator is added in the second step, and the stirring is carried out for 20-30 min.
4. The method of claim 2 wherein the second step is performed by adding tetramethylammonium polyhedral oligomeric silsesquioxane at a temperature of 15 ℃.
5. The method for preparing the low-temperature guar gel breaker for oil and gas well fracturing as claimed in claim 2, wherein polyethylene glycol is added in the third step, and stirring is carried out for 1.5 h.
6. The method for preparing the low-temperature guar gel breaker for oil and gas well fracturing as claimed in claim 2, wherein the third step is carried out at room temperature below 15 ℃.
7. A fracturing fluid comprising the low temperature guar breaker of claim 1 for fracturing oil and gas wells.
8. A method for increasing the yield and the injection of an oil-water well, which is characterized by using the fracturing fluid of claim 7.
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