CN114806521B - Preparation method of shear thickening temporary plugging agent, plugging agent and evaluation method - Google Patents
Preparation method of shear thickening temporary plugging agent, plugging agent and evaluation method Download PDFInfo
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Abstract
The invention discloses a preparation method of a shear thickening temporary plugging agent, the temporary plugging agent and an evaluation method. The preparation method comprises the following steps: adding alcohol and deionized water into ethyl silicate, and dripping ammonia water into the ethyl silicate to obtain a solution A; step (2), stirring and hydrolyzing amino polyethylene glycol and a silane coupling agent to obtain a solution B; and (3) slowly dripping the solution B into the solution A, adding a catalyst, stirring, performing hydrolysis reaction to obtain a viscous solution, and cooling to obtain the shear thickening plugging agent. The temporary plugging agent can reduce the volume of the temporary plugging agent and is also beneficial to improving the temporary plugging efficiency. According to the evaluation method, the temporary plugging agent is evaluated according to the performance of the shear thickening material, the performance of the temporary plugging agent is known through evaluation parameters, the construction design of shale fracturing is guided, and the applicable temporary plugging agent is selected to control the morphology of a shale fracture network, so that the single-well productivity of shale gas is improved.
Description
Technical Field
The invention relates to the technical field of drilling, in particular to a preparation method, a plugging agent and an evaluation method of a shear thickening temporary plugging agent.
Background
At present, conventional temporary plugging agents have been widely used in hydraulic fracturing construction. The method aims at temporarily plugging at a certain position in the crack, so that the net pressure in the crack is promoted to quickly rise, and then the branch crack or the micro-crack is pushed open, and finally the complexity degree and the reconstruction volume of the crack are improved. Or temporarily plugging the pressed-out interval, and further pressing-out the interval with higher stress along with the continuous rising of the pressure of the shaft. It can be said that the temporary plugging agent can greatly improve the longitudinal fracture opening degree and the fracture steering effect on the plane.
However, the temporary plugging agent has technical limitations, such as relatively long glue forming time, so that the amount of the temporary plugging agent required in temporary plugging is large, thereby not only bringing about rapid rise of cost, but also bringing about certain challenges for thoroughly breaking glue after pressing. In addition, when the horizontal well is subjected to staged multi-cluster fracturing, the pressure gradient exists in the flowing process of the horizontal well, the propping agent is moved and the flowing following property of the fracturing fluid is poor, and the like, so that the extension degree of each cluster of cracks is uneven, the induced stress exists on the basis of balanced extension of each cluster of cracks, otherwise, a part of cracks are unique and elegant, correspondingly, the absorbed fracturing fluid volume ratio is maximum, the induced stress is also maximum, and the cracking and extension of other cracks with relatively weak extension degree are prevented. However, although the conventional temporary plugging agent is easy to plug cracks with large extension degree, the temporary plugging agent has relatively long gelling time, temporary plugging of the seam and temporary plugging in the seam cannot be considered, and the volume of the wasted temporary plugging agent cannot be avoided.
Chinese patent CN108612507a discloses a method for temporary plugging and diverting fracturing using shear thickening fluid STF as temporary plugging agent. The shearing thickening fluid has the characteristic of increasing viscosity under high-speed shearing, and can be used as a temporary plugging agent to adaptively improve the viscosity of the fluid temporary plugging agent at the early stage of flowing, so that the volume of the temporary plugging agent can be correspondingly reduced, and the temporary plugging efficiency can be improved.
Chinese patent CN109233783a relates to a shear thickening liquid, modified degradable fiber based on the same, preparation method and temporary plugging steering fracturing method: preparing a shear thickening liquid; secondly, modifying the degradable fiber DF-1; thirdly, setting a fracturing packer, and injecting a front hydraulic fracturing stratum; fourthly, injecting sand-carrying fluid mixed with the modified degradable fiber to fill the crack; fifth, injecting fiber steering agent solution to steer and make a seam; and step six, injecting sand-carrying fluid mixed with modified degradable fibers into the new joint to fill, and then displacing and stopping the pump. According to the invention, the non-Newtonian fluid is utilized to modify the degradable fiber DF-1, so that a reticular structure formed by the fiber in the solution is more stable, and the temporary plugging capability of the fiber in the stratum fracture is greatly enhanced; compared with the prior art, the method can make more deeper branch joints, greatly improve the connectivity of old joints, natural joints and unused reservoir areas, and is suitable for popularization and use in low-permeability dense reservoirs.
However, only the conventional method for evaluating the temporary plugging agent is adopted at present, and no method for evaluating the performance of the shear thickening fluid as the temporary plugging agent is adopted.
Therefore, a novel shearing temporary plugging agent and a performance evaluation method of the temporary plugging agent are required to be researched and proposed, so that the shearing thickening fluid is systematically, effectively, quantitatively and accurately evaluated as the temporary plugging agent to realize the temporary plugging effect in the joint.
Disclosure of Invention
The invention provides a preparation method of a shear thickening temporary plugging agent, a plugging agent and an evaluation method for solving the problems in the prior art. Aiming at the performance characteristics of the shear thickening fluid as a temporary plugging agent, the invention systematically, effectively, quantitatively and accurately evaluates the shear thickening fluid as the temporary plugging agent to realize the temporary plugging effect in the joint. The invention has the advantage of being capable of accurately, objectively and effectively evaluating the difference of the shear thickening fluid serving as the temporary plugging agent from the conventional temporary plugging agent.
The invention aims at providing a preparation method of a shear thickening temporary plugging agent.
The method comprises the following steps:
step (1), mixing ethyl silicate, alcohol, water and ammonia water to obtain a solution A;
step (2), stirring and hydrolyzing amino polyethylene glycol and a silane coupling agent to obtain a solution B;
and (3) slowly dripping the solution B into the solution A, adding a catalyst, stirring, performing hydrolysis reaction to obtain a viscous solution, and cooling to obtain the shear thickening plugging agent.
In a preferred embodiment of the present invention,
in the step (1), the step of (a),
the volume ratio of the ethyl silicate to the alcohol to the water to the ammonia water is as follows: 1: (1-1.6): (1-1.8): (0.02-0.1);
the alcohol is one or a combination of ethanol, propanol, isopropanol, tertiary butanol, n-butanol or ethylene glycol.
The water is preferably deionized water; the ammonia water is conventional concentrated ammonia water in the prior art;
the mixing mode of the ethyl silicate, the alcohol, the water and the ammonia water can be a conventional mixing mode, and the mixture is uniformly mixed. The technical staff can determine according to the actual situation, and can mix the ethyl silicate, the alcohol and the water firstly and then drip the ammonia water; or mixing ethyl silicate and alcohol to form solution a, mixing water and ammonia water to form solution b, and dripping solution b into solution a.
In a preferred embodiment of the present invention,
in the step (2), the step of (C),
the molecular weight of the amino polyethylene glycol is more than or equal to 50 ten thousand;
the mass ratio of the amino polyethylene glycol to the silane coupling agent is 1: (0.001-0.03).
In a preferred embodiment of the present invention,
the hydrolysis reaction temperature in the step (2) is 45-55 ℃.
In a preferred embodiment of the present invention
In the step (3), the step of (c),
the catalyst is acetic acid or alkali;
the dosage of the catalyst is 0.1% -3% of the sum of the mass of the solution A and the mass of the solution B;
in a preferred embodiment of the present invention
Step (3),
the mass ratio of the solution A to the solution B is (0.2-1): 1.
in a preferred embodiment of the present invention,
step (3),
the hydrolysis reaction temperature is 50-60 ℃; the hydrolysis reaction time is 2-6h.
The second object of the invention is to provide a shear thickening temporary plugging agent obtained by the method.
The invention further provides an evaluation method of the shear thickening temporary plugging agent.
The evaluation method includes:
1) Determining physical simulation parameters of 2-layer vertical well and 2-cluster horizontal well staged fracturing;
2) A shear sensitivity evaluation experiment of the shear thickening temporary plugging agent;
3) Breaking gel of the shear thickening temporary plugging agent;
4) Crack initiation and object model expansion experiments under the action of no temporary plugging agent;
5) Crack initiation and object model expansion experiments under the action of conventional temporary plugging agents;
6) Crack initiation and extension object model experiment under the action of shear thickening temporary plugging agent;
7) The expansion proportion of the cracks is adjusted by adjusting the dosage and the injection mode of the shear thickening temporary plugging agent, and the difference of the expansion lengths of the cracks at two sides is less than 10%.
The invention adopts the following technical scheme:
the preparation method of the shear thickening temporary plugging agent comprises the following specific steps:
1) Adding a certain amount of alcohol and deionized water into the calculated amount of TEOS, and dripping the calculated amount of ammonia water to obtain solution A.
The alcohol comprises one or a mixture of several of ethanol, propanol, isopropanol, tert-butanol, n-butanol or ethylene glycol, preferably ethanol.
2) The calculated amount of aminopolyethylene glycol and the silane coupling agent are hydrolyzed under stirring at 50 ℃ to obtain a solution B.
3) Slowly dropwise adding the calculated amount B into the A, adding a small amount of acetic acid or alkali as a catalyst, stirring, carrying out hydrolysis reaction for 2-6h at 50-60 ℃ to obtain a viscous solution, and cooling the system to room temperature to obtain a shearing thickening solution;
the amino polyethylene glycol comprises one or more of single end and double end, and has molecular weight of 50 ten thousand or more, such as 50 ten thousand, 55 ten thousand, 60 ten thousand, 65 ten thousand, 70 ten thousand, 80 ten thousand, 100 ten thousand, 120 ten thousand, 150 ten thousand, 180 ten thousand, 200 ten thousand or more.
The silane coupling agent includes typical silane coupling agents such as one or a mixture of several of A151, A171, A172, KH560, KH561, KH570, SCA903, DL602, DL171, preferably KH560 and KH561.
The mass ratio of the amino polyethylene glycol to the silane coupling agent is 1: (0.001-0.03).
The evaluation method of the shear thickening temporary plugging agent comprises the following specific steps:
and determining the physical simulation parameters of the 2-layer and 2-cluster staged fracturing of the vertical well. The conditions of temperature, pressure and the like in the field are considered as far as possible by utilizing similar principles. For this purpose, a corresponding simulation can be performed on a dual cluster fracture initiation and propagation simulation device. The simulated core size of the physical simulation device is 300mm gamma and 600mm gamma. Different ground stresses can be applied in three directions, and layered stresses can also be applied in layers (5 layers of ground stresses can be applied in layers to simulate the crack initiation and extension rules of 2 layers). The highest loading stress was 30mpa and the temperature was 120 ℃. In addition, the vertical well bore can simulate both a 2-layer vertical well and a 2-cluster horizontal well by applying different correspondences. The difference is that the perforation mode is different, the vertical well can be produced according to spiral perforation, the horizontal well can adopt a plane perforation mode, and the horizontal comparison analysis can be carried out by adopting spiral perforation. (the fracture convexity and concavity can be analyzed by a three-dimensional appearance instrument on the fracture surface after pressing, in general, the higher the viscosity of the fracturing fluid, the smoother the fracture surface which extends after the core is broken, and the lower the fracture convexity and concavity, and vice versa. In order to distinguish the shear thickening temporary plugging agent from the rest of the fracturing fluid, the temporary plugging agent may be dyed. And designing crack initiation and expansion physical simulation research under different parameter combinations under two conditions by combining the temperature and pressure conditions of a specific target well layer. Firstly, based on various rock mechanical parameters, physical properties and the like of a rock core, an artificial rock sample with similar properties is prepared.
For vertical well zone fracturing, the stress difference between 2 layers can be respectively designed to be 1-3-5-7mpa, and the stress of the middle interlayer can be set to be constant, such as 20mpa, and for simplicity, the stress difference of each storage interlayer can be respectively 1-3-5-7mpa; for horizontal well 2 cluster fracturing, the perforation diameters may or may not be equal, whether spiral or planar. In order to promote the balanced extension of 2 clusters of cracks, different hole numbers can be arranged on plane perforation, for example, 1-2-3-4 perforations are respectively arranged on each plane, so as to observe the crack initiation and extension rules under different perforation cluster numbers.
The viscosity of the fracturing fluid can be respectively designed to be 1-5-10-20-50mpa.s, and 3 types of displacement can be set according to the principle of linear velocity similarity, namely, low-medium-high three types of displacement.
And setting parameters of the shear thickening temporary plugging agent based on the volume ratio of the fracturing fluid of the specific target well layer to the temporary plugging agent. However, the viscosity ratio may be 1:1, designing.
3) Shear sensitivity evaluation experiment of shear thickening temporary plugging agent
The shear rate history of the target well is simulated by using a conventional rheometer under three conditions of well bore, perforation, crack and the like, and particularly the viscosity increase condition under the condition of simulating perforation eye high shear rate (the shear time can be 3-5 min). In order to increase the effect of shear thickening, the viscosity should be increased by more than 50%, otherwise, the step 1) can be returned to carry out the molecular structure design of the polymer of the temporary plugging agent for shear thickening again.
4) Gel breaking experiment of shear thickening temporary plugging agent
Based on the temperature field simulation result of the target well layer fracturing, adding ammonium persulfate gel breakers with different concentrations (microcapsule coated ammonium persulfate and uncoated ammonium persulfate with different proportions can be designed) under the temperature fields of different construction stages, and testing the viscosity of the shear thickening temporary plugging agent after gel breaking in different time, wherein the viscosity is higher than 5map.s, so that the higher gel breaker concentration is set. Until an optimized breaker concentration is obtained.
5) Crack initiation and propagation object model experiment without temporary plugging agent
Based on the parameters of the step 2), experimental study on crack initiation and propagation conditions under different parameter combinations is carried out.
6) Crack initiation and expansion object model experiment under conventional temporary plugging agent effect
Based on the step 2), carrying out crack initiation and propagation object model experiments under different conditions by using the parameters of the step 2) and the conventional dyeing temporary plugging agent. Especially, when the temporary plugging agent is used for fracturing multiple layers in the vertical well and the horizontal well is used for fracturing the clusters, the extension uniformity degree of each cluster of cracks is compared.
The volume of the conventional temporary plugging agent can be relatively high in consideration of the fact that the viscosity of the conventional temporary plugging agent is equal to low.
7) Crack initiation and extension object model experiment under action of shear thickening temporary plugging agent
Step 5) is repeated, except that the newly developed dyed shear thickening temporary plugging agent is replaced. Considering that the viscosity is relatively higher, the volume of the temporary plugging agent can be smaller than that of a conventional temporary plugging agent.
8) Comparing the crack propagation conditions of step 7) and step 6). If the difference between the two is more than 10% (the uniformity of crack propagation of the vertical well stratified fracturing and the horizontal well stratified fracturing), the viscosity of the shear thickening temporary plugging agent is adjusted, then the crack propagation proportion under the action of the shear thickening temporary plugging agent is tested (the step 1), the step 7) and the step 8) are repeated until the difference between the two results is less than 10%.
ADVANTAGEOUS EFFECTS OF INVENTION
The temporary plugging agent can reduce the volume of the temporary plugging agent and is also beneficial to improving the temporary plugging efficiency. The invention also provides a method for evaluating the performance of the shear thickening temporary plugging agent, which is different from the method for evaluating the general temporary plugging agent, the performance of the temporary plugging agent is evaluated according to the performance of the shear thickening material, the performance of the temporary plugging agent is known through evaluation parameters, the construction design of shale fracturing is guided, and the applicable temporary plugging agent is selected to control the morphology of a shale fracture network, so that the single-well productivity of the shale gas is improved.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
All materials in the examples are commercially available.
Preparation of a shear thickening temporary plugging agent:
example 1:
(1) TEOS and ethanol are added to form a solution a; deionized water and strong ammonia water to form solution b. And adding the solution b into the solution a at the temperature of 50 ℃ to react for 2 hours to obtain a solution A. The volume ratio of the ethyl silicate to the ethanol to the deionized water to the ammonia water is as follows: 1:1:1:0.02;
(2) diamino polyethylene glycol (molecular weight is 80 ten thousand) and a silane coupling agent KH560 are hydrolyzed according to a mass ratio of 1:0.001 under the stirring condition of 50 ℃ to obtain a solution B.
(3) Slowly dripping B into A, wherein the mass ratio of B to A is 1:1, and adding acetic acid as a catalyst, wherein the dosage of the catalyst is 0.1% of the sum of the mass of the solution A and the mass of the solution B; and (3) carrying out hydrolysis reaction for 4 hours at 50 ℃ to obtain a viscous solution, and cooling the system to room temperature to obtain the shear thickening temporary plugging agent.
Example 2
(1) TEOS and ethanol are added to form a solution a; deionized water and strong ammonia water to form solution b. And adding the solution b into the solution a at the temperature of 50 ℃ to react for 2 hours to obtain a solution A. The volume ratio of the ethyl silicate to the ethanol to the deionized water to the ammonia water is as follows: 1:1.6:1.8:0.1;
(2) diamino polyethylene glycol (molecular weight is 100 ten thousand) and a silane coupling agent KH560 are hydrolyzed according to the mass ratio of 1:0.03 under the stirring condition of 45 ℃ to obtain a solution B.
(3) Slowly dripping B into A, wherein the mass ratio of B to A is 1:0.2, adding acetic acid as a catalyst, wherein the dosage of the catalyst is 3% of the sum of the mass of the solution A and the mass of the solution B, carrying out hydrolysis reaction for 6 hours at 60 ℃, obtaining a viscous solution, and cooling the system to room temperature to obtain the shear thickening temporary plugging agent.
Example 3
(1) TEOS and ethanol are added to form a solution a; deionized water and strong ammonia water to form solution b. Adding the solution b into the solution a at the temperature of 50 ℃ for 2h to obtain a solution A; the volume ratio of the ethyl silicate to the ethanol to the deionized water to the ammonia water is as follows: 1:1.2:1.5:0.08;
(2) diamino polyethylene glycol (molecular weight is 120 ten thousand) and a silane coupling agent KH560 are hydrolyzed according to a mass ratio of 1:0.01 under the stirring condition of 55 ℃ to obtain a solution B.
(3) Slowly dripping B into A, wherein the mass ratio of B to A is 1:0.5, and adding acetic acid as a catalyst, wherein the dosage of the catalyst is 2% of the sum of the mass of the solution A and the mass of the solution B; and (3) carrying out hydrolysis reaction for 5 hours at 55 ℃ to obtain a viscous solution, and cooling the system to room temperature to obtain the shear thickening temporary plugging agent.
Example 4 evaluation method of temporary blocking agent
1) The shear thickening temporary plugging agent prepared in example 1 is adopted
2) Staged fracturing physical simulation parameter determination
The stress of the barrier layer was designed to be 20mpa and the reservoir stress was divided into 19mpa and 17mpa, i.e., the stress difference was 1mpa and 3mpa. A spiral perforation mode is adopted. The viscosity of the fracturing fluid is 10-20-50mpa.s, the displacement is 5ml/min,10ml/min and 20ml/min respectively.
3) Shear sensitivity evaluation experiment of shear thickening temporary plugging agent
Rheometer at 170 -1 And shearing for 5min at the rotating speed of s, and observing the viscosity change of the shear thickening temporary plugging agent. The shear thickening temporary plugging agent is increased from the initial 160mpa.s to 265mpa.s, and the amplification reaches 65.6%.
4) Gel breaking experiment of shear thickening temporary plugging agent
And adding 0.05% of ammonium persulfate gel breaker at 120 ℃, testing the viscosity of the shear thickening temporary plugging agent after gel breaking within 2 hours, wherein the viscosity of the gel breaking solution is 3mpa.s after testing.
5) The experimental study of the crack initiation and the expansion object model without the temporary plugging agent is shown in the table 1.
TABLE 1
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 10mPa·s | 0.075/0.062 |
| 2 | 10ml/min | 10mPa·s | 0.083/0.07 |
| 3 | 20ml/min | 10mPa·s | 0.112/0.089 |
| 4 | 5ml/min | 20mPa·s | 0.084/0.067 |
| 5 | 10ml/min | 20mPa·s | 0.117/0.087 |
| 6 | 20ml/min | 20mPa·s | 0.137/0.109 |
| 7 | 5ml/min | 50mPa·s | 0.092/0.067 |
| 8 | 10ml/min | 50mPa·s | 0.124/0.101 |
| 9 | 20ml/min | 50mPa·s | 0.147/0.115 |
Crack propagation uniformity is greater than 10%.
6) The data of the crack initiation and expansion object model experiment under the action of the conventional temporary plugging agent are shown in table 2.
TABLE 2
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 10mPa·s | 0.072/0.063 |
| 2 | 10ml/min | 10mPa·s | 0.081/0.072 |
| 3 | 20ml/min | 10mPa·s | 0.108/0.096 |
| 4 | 5ml/min | 20mPa·s | 0.081/0.072 |
| 5 | 10ml/min | 20mPa·s | 0.113/0.094 |
| 6 | 20ml/min | 20mPa·s | 0.131/0.117 |
| 7 | 5ml/min | 50mPa·s | 0.089/0.072 |
| 8 | 10ml/min | 50mPa·s | 0.12/0.108 |
| 9 | 20ml/min | 50mPa·s | 0.142/0.124 |
Crack propagation uniformity is greater than 10%.
7) The data of the crack initiation and extension modulus experiment under the action of the shear thickening temporary plugging agent of the example 1 are shown in table 3.
TABLE 3 Table 3
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 10mPa·s | 0.0705/0.065 |
| 2 | 10ml/min | 10mPa·s | 0.078/0.074 |
| 3 | 20ml/min | 10mPa·s | 0.105/0.096 |
| 4 | 5ml/min | 20mPa·s | 0.078/0.072 |
| 5 | 10ml/min | 20mPa·s | 0.109/0.099 |
| 6 | 20ml/min | 20mPa·s | 0.128/0.116 |
| 7 | 5ml/min | 50mPa·s | 0.086/0.079 |
| 8 | 10ml/min | 50mPa·s | 0.116/0.107 |
| 9 | 20ml/min | 50mPa·s | 0.139/0.128 |
Crack propagation uniformity is less than 10%, meeting the required performance.
Example 5 method for evaluating temporary blocking agent
1) The shear thickening temporary plugging agent prepared in example 2
2) Determination of physical simulation parameters for fracture
The stress of the barrier layer is designed to be 15mpa and the reservoir stress is divided into 12mpa and 20mpa, i.e. the stress difference is 3mpa and 5mpa. A spiral perforation mode is adopted. The viscosity of the fracturing fluid is 1-5-10mpa.s, the displacement is 5ml/min,10ml/min and 15ml/min respectively.
3) Shear sensitivity evaluation experiment of shear thickening temporary plugging agent
Rheometer at 170 -1 And shearing for 5min at the rotating speed of s, and observing the viscosity change of the shear thickening temporary plugging agent. The shear thickening temporary plugging agent is increased from the initial 120mpa.s to 210mpa.sThe web reached 75%.
4) Gel breaking experiment of shear thickening temporary plugging agent
And adding 0.05% of ammonium persulfate gel breaker at 120 ℃, testing the viscosity of the shear thickening temporary plugging agent after gel breaking within 2 hours, wherein the viscosity of the gel breaking solution is 6mpa.s after testing.
5) The experimental study of the crack initiation and the expansion object model without the temporary plugging agent is shown in the table 4.
TABLE 4 Table 4
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 1mPa·s | 0.077/0.061 |
| 2 | 10ml/min | 1mPa·s | 0.082/0.067 |
| 3 | 15ml/min | 1mPa·s | 0.089/0.071 |
| 4 | 5ml/min | 5mPa·s | 0.083/0.064 |
| 5 | 10ml/min | 5mPa·s | 0.096/0.072 |
| 6 | 15ml/min | 5mPa·s | 0.108/0.089 |
| 7 | 5ml/min | 10mPa·s | 0.088/0.074 |
| 8 | 10ml/min | 10mPa·s | 0.097/0.083 |
| 9 | 15ml/min | 10mPa·s | 0.106/0.091 |
Crack propagation uniformity is greater than 10%.
6) The data of the crack initiation and expansion object model experiment under the action of the conventional temporary plugging agent are shown in table 5.
TABLE 5
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 1mPa·s | 0.075/0.066 |
| 2 | 10ml/min | 1mPa·s | 0.079/0.072 |
| 3 | 15ml/min | 1mPa·s | 0.084/0.076 |
| 4 | 5ml/min | 5mPa·s | 0.078/0.07 |
| 5 | 10ml/min | 5mPa·s | 0.089/0.081 |
| 6 | 15ml/min | 5mPa·s | 0.096/0.092 |
| 7 | 5ml/min | 10mPa·s | 0.084/0.079 |
| 8 | 10ml/min | 10mPa·s | 0.092/0.087 |
| 9 | 15ml/min | 10mPa·s | 0.101/0.096 |
Crack propagation uniformity is greater than 10%.
7) The data of the crack initiation and extension modulus experiment under the action of the shear thickening temporary plugging agent of the embodiment 2 are shown in table 6.
TABLE 6
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 1mPa·s | 0.072/0.069 |
| 2 | 10ml/min | 1mPa·s | 0.076/0.074 |
| 3 | 15ml/min | 1mPa·s | 0.081/0.078 |
| 4 | 5ml/min | 5mPa·s | 0.08/0.072 |
| 5 | 10ml/min | 5mPa·s | 0.086/0.084 |
| 6 | 15ml/min | 5mPa·s | 0.094/0.093 |
| 7 | 5ml/min | 10mPa·s | 0.082/0.08 |
| 8 | 10ml/min | 10mPa·s | 0.09/0.089 |
| 9 | 15ml/min | 10mPa·s | 0.99/0.098 |
Crack propagation uniformity is less than 10%, meeting the required performance.
Example 6 method for evaluating temporary blocking agent
1) The shear thickening temporary plugging agent prepared in example 3
2) Staged fracturing physical simulation parameter determination
The stress of the designed interlayer is 16/20/32mpa, and the stress of the reservoir is divided into 16mpa, 25mpa and, namely, the stress difference is 1/3/5/7mpa. A spiral 5 perforation mode is adopted. The viscosity of the fracturing fluid is 5-10-20mpa.s, the displacement is 5ml/min,10ml/min and 20ml/min respectively.
3) Shear sensitivity evaluation experiment of shear thickening temporary plugging agent
Rheometer at 170 -1 And shearing for 5min at the rotating speed of s, and observing the viscosity change of the shear thickening temporary plugging agent. The shear thickening temporary plugging agent is increased from original 220mpa.s to 340mpa.s, and the increase reaches 54.6%.
4) Gel breaking experiment of shear thickening temporary plugging agent
And adding 0.05% of ammonium persulfate gel breaker at 120 ℃, testing the viscosity of the shear thickening temporary plugging agent after gel breaking within 2 hours, wherein the viscosity of the gel breaking solution is 6mpa.s after testing.
5) The experimental study of the crack initiation and the expansion object model without the temporary plugging agent is shown in Table 7.
TABLE 7
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 5mPa·s | 0.071/0.055 |
| 2 | 10ml/min | 5mPa·s | 0.078/0.062 |
| 3 | 20ml/min | 5mPa·s | 0.095/0.074 |
| 4 | 5ml/min | 10mPa·s | 0.077/0.06 |
| 5 | 10ml/min | 10mPa·s | 0.102/0.072 |
| 6 | 20ml/min | 10mPa·s | 0.116/0.089 |
| 7 | 5ml/min | 20mPa·s | 0.087/0.0.063 |
| 8 | 10ml/min | 20mPa·s | 0.118/0.92 |
| 9 | 20ml/min | 20mPa·s | 0.126/0.105 |
Crack propagation uniformity is greater than 10%.
6) The data of the crack initiation and expansion object model experiment under the action of the conventional temporary plugging agent are shown in Table 8.
TABLE 8
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 5mPa·s | 0.068/0.057 |
| 2 | 10ml/min | 5mPa·s | 0.075/0.063 |
| 3 | 20ml/min | 5mPa·s | 0.092/0.076 |
| 4 | 5ml/min | 10mPa·s | 0.079/0.063 |
| 5 | 10ml/min | 10mPa·s | 0.098/0.078 |
| 6 | 20ml/min | 10mPa·s | 0.109/0.092 |
| 7 | 5ml/min | 20mPa·s | 0.084/0.0.068 |
| 8 | 10ml/min | 20mPa·s | 0.112/0.95 |
| 9 | 20ml/min | 20mPa·s | 0.121/0.108 |
Crack propagation uniformity is greater than 10%.
7) The data of the crack initiation and extension modulus experiment under the action of the shear thickening temporary plugging agent of the embodiment 3 are shown in table 9.
TABLE 9
| Sequence number | Displacement volume | Viscosity of fracturing fluid | Crack propagation ratio |
| 1 | 5ml/min | 5mPa·s | 0.066/0.059 |
| 2 | 10ml/min | 5mPa·s | 0.078/0.066 |
| 3 | 20ml/min | 5mPa·s | 0.088/0.079 |
| 4 | 5ml/min | 10mPa·s | 0.076/0.068 |
| 5 | 10ml/min | 10mPa·s | 0.092/0.083 |
| 6 | 20ml/min | 10mPa·s | 0.104/0.096 |
| 7 | 5ml/min | 20mPa·s | 0.08/0.0.072 |
| 8 | 10ml/min | 20mPa·s | 0.106/0.97 |
| 9 | 20ml/min | 20mPa·s | 0.117/0.112 |
Crack propagation uniformity is less than 10%, meeting the required performance.
Claims (6)
1. A method for preparing a shear thickening temporary plugging agent, which is characterized by comprising the following steps:
step (1), mixing ethyl silicate, alcohol, water and ammonia water to obtain a solution A;
the volume ratio of the ethyl silicate to the alcohol to the water to the ammonia water is as follows: 1: (1-1.6): (1-1.8): (0.02-0.1);
the alcohol is one or a combination of ethanol, propanol, isopropanol, tertiary butanol, n-butanol or ethylene glycol;
step (2), stirring and hydrolyzing amino polyethylene glycol and a silane coupling agent to obtain a solution B;
the molecular weight of the amino polyethylene glycol is more than or equal to 50 ten thousand;
the mass ratio of the amino polyethylene glycol to the silane coupling agent is 1: (0.001-0.03);
the amino polyethylene glycol is diamino polyethylene glycol;
the silane coupling agent is one or a mixture of more of KH560, KH561 and KH 570;
step (3) slowly dripping the solution B into the solution A, adding a catalyst, stirring, performing hydrolysis reaction to obtain a viscous solution, and cooling to obtain a shear thickening plugging agent;
the mass ratio of the solution A to the solution B is (0.2-1): 1.
2. the method of manufacturing according to claim 1, wherein:
the reaction temperature of the hydrolysis in the step (2) is 45-55 ℃.
3. The method of manufacturing according to claim 1, wherein:
in the step (3), the step of (c),
the catalyst is acetic acid or alkali;
the dosage of the catalyst is 0.1% -3% of the sum of the mass of the solution A and the mass of the solution B.
4. The method of manufacturing according to claim 1, wherein:
in the step (3), the step of (c),
the temperature of the hydrolysis reaction is 50-60 ℃; the hydrolysis reaction time is 2-6h.
5. A shear thickening temporary plugging agent obtainable by the process of any one of claims 1 to 4.
6. A method of evaluating a shear thickening temporary plugging agent according to claim 5, characterized in that said evaluation method comprises:
1) Determining physical simulation parameters of 2-layer vertical well and 2-cluster horizontal well staged fracturing;
2) A shear sensitivity evaluation experiment of the shear thickening temporary plugging agent;
3) Breaking gel of the shear thickening temporary plugging agent;
4) Crack initiation and object model expansion experiments under the action of no temporary plugging agent;
5) Crack initiation and object model expansion experiments under the action of conventional temporary plugging agents;
6) Crack initiation and extension object model experiment under the action of shear thickening temporary plugging agent;
7) The expansion proportion of the cracks is adjusted by adjusting the dosage and the injection mode of the shear thickening temporary plugging agent, and the difference of the expansion lengths of the cracks at two sides is less than 10%.
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| US4663366A (en) * | 1983-07-25 | 1987-05-05 | Exxon Research & Engineering Company | Shear thickening composition with polycarboxylic acid |
| CN101157745A (en) * | 2007-09-11 | 2008-04-09 | 浙江大学 | Method for grafting polymer on inorganic material surface |
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| US20160319185A1 (en) * | 2013-12-18 | 2016-11-03 | Schlumberger Technology Corporation | Shear thickening fluid method and system to deliver materials downhole |
| EP3541889A1 (en) * | 2016-11-15 | 2019-09-25 | Saudi Arabian Oil Company | Nanoparticle-based shear-thickening materials |
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| CN101157745A (en) * | 2007-09-11 | 2008-04-09 | 浙江大学 | Method for grafting polymer on inorganic material surface |
| CN108612507A (en) * | 2018-04-16 | 2018-10-02 | 西安石油大学 | A method of carrying out temporarily stifled turnaround fracture using shear thickening liquid |
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