CN115612481B - Slow-release guar gum fracturing fluid gel breaker and preparation method thereof - Google Patents
Slow-release guar gum fracturing fluid gel breaker and preparation method thereof Download PDFInfo
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- CN115612481B CN115612481B CN202211546483.6A CN202211546483A CN115612481B CN 115612481 B CN115612481 B CN 115612481B CN 202211546483 A CN202211546483 A CN 202211546483A CN 115612481 B CN115612481 B CN 115612481B
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to the field of oilfield chemical fracturing fluids, and particularly relates to a sustained-release guar gum fracturing fluid gel breaker and a preparation method thereof. The sustained-release gel breaker adopts high-strength hollow ceramsite microspheres as a carrier, bears crystals obtained after vacuum drying of an ammonium persulfate aqueous solution, and the surfaces of the hollow ceramsite microspheres are coated with a brittle resin material and a dispersing agent. The sustained-release guar gum fracturing fluid gel breaker provided by the invention has the advantages of low cost, strong bearing capacity, simple manufacturing process, controlled release effect and reliable gel breaking delaying effect.
Description
Technical Field
The invention belongs to the field of oilfield chemical fracturing fluids, and particularly relates to a sustained-release guar gum fracturing fluid gel breaker and a preparation method thereof.
Background
The water-based fracturing construction operation needs to add a gel breaker into the fracturing fluid so as to degrade polymers in the fracturing fluid after fracturing is finished, and flowback is facilitated. However, the conventional gel breaker is easy to lose a large amount in the pumping process, the gel breaking effect is reduced, if the high-concentration gel breaker is adopted, the fracturing fluid is broken in advance, and sand carrying is not facilitated, and in recent years, the capsule gel breaker aiming at the problem generally has the problems of low bearing capacity, easy release in advance, complex manufacturing process, high cost and the like. Guo Gang, zhao Zhenfeng, etc. by using propping agent ceramsite, resin binder, curing agent and gel breaker, a coated propping agent with slow-release gel-breaking function for fracturing fluid is developed, which is composed of a three-layer composite structure, and comprises a slow-release layer, a gel-breaking layer and a propping agent from outside to inside in sequence. CN 110055048A integrates the functions of bearing, slowly releasing gel breaker and supporting cracks, but the gel breaker layer is an annulus between the proppant and the slowly releasing layer, the space is small, the gel breaker bearing dosage is low, the pressure bearing capacity of the annulus gel breaker layer is poor, and the gel breaker is easily released in advance. CN 104031628A an ammonium persulfate gel breaker is sealed in ethyl cellulose porous microspheres by an ionic emulsifier and a hot-melt material to prepare the ultramicro capsule type gel breaker, and the particle size of the ultramicro capsule type gel breaker is less than 50 mu m. Due to the fact that the particle size is too small, the gel breaker is difficult to break under the action of crack closing stress, and therefore the gel breaker is difficult to release in time to exert gel breaking effect.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a sustained-release guar gum fracturing fluid gel breaker and a preparation method thereof.
The invention relates to a sustained-release guar gum fracturing fluid gel breaker, which adopts high-strength hollow ceramsite microspheres as a carrier, bears crystals obtained after ammonium persulfate aqueous solution is dried in vacuum, and the surfaces of the hollow ceramsite microspheres are coated with brittle resin materials and dispersing agents.
The strength of the high-strength hollow ceramsite microspheres is 23-30Mpa, and the high-strength hollow ceramsite microspheres are preferably prepared by the method disclosed in Chinese patent 201710473085.9. The hollow ceramsite microspheres have good pressure-bearing capacity, and can prevent the capsule core of the gel breaker from being released in advance during the injection of a fracturing fluid pump. The gel breaker is not released in the pumping process, so that the pumping construction is ensured, and the microspheres are broken to release the gel breaker only after the crack closing stress is applied.
The brittle resin material is preferably resin, more preferably epoxy resin or SR762 type acrylic resin or E0578 type acrylic resin or a mixture thereof; the dispersing agent is nano calcium carbonate powder.
The preparation method comprises the following specific steps:
(1) Dissolving ammonium persulfate in distilled water to obtain an ammonium persulfate aqueous solution;
(2) Adding hollow ceramsite microspheres into an ammonium persulfate aqueous solution until the hollow ceramsite microspheres are just immersed, and then drying and crystallizing in vacuum to obtain loaded microspheres;
(3) And adding a mixture containing a brittle resin material into the loaded microspheres, stirring, adding a dispersing agent, stirring, standing, and screening to obtain a finished product.
In the step (1), the mass fraction of the ammonium persulfate solution is 27-35%;
in the step (2), the mass ratio of the hollow ceramsite microspheres to the ammonium persulfate aqueous solution is 2.2:1 to 3:1.
in the step (2), the vacuum drying temperature is 70-75 ℃, and the drying time is 24h. Vacuum drying is carried out at 70-75 ℃, so that the gel breaking performance of the ammonium persulfate can be greatly maintained, and the effect of quickly drying moisture for crystallization in a short time can be achieved. Above this temperature, the drying time is significantly reduced, but the gel breaking properties of the resulting product are also affected. If the temperature is lower than the temperature range, the drying time can be greatly prolonged, and the gel breaking performance of the product (compared with vacuum drying at 70-75 ℃) can not be obviously improved.
In the step (3), the dosage of the mixture containing the brittle resin material is 15-25% of the mass of the loaded microsphere.
In the step (3), when the resin is acrylic resin, the mixture containing the brittle resin material is a mixture of the resin and absolute ethyl alcohol, and the mass ratio of the resin: absolute ethanol =1:4. when the epoxy resin is adopted, the mixture containing the brittle resin material is a mixture of the resin and a curing agent, and the mass ratio of the resin: curing agent =4:1.
in the step (3), the mixing time is 5min, the stirring time is 5min, and the standing time is 24h.
The sustained-release guar gum fracturing fluid gel breaker can be added in the process of adding sand into fracturing fluid, and the dosage of the gel breaker can be in reference to the conventional capsule gel breaker and can also be matched with ammonium persulfate for use.
The method has the beneficial effects that after the solid matter obtained by vacuum drying of the ammonium persulfate solution is verified to still have good gel breaking efficiency, the method abandons the bearing way of the conventional encapsulated gel breaker on the ammonium persulfate gel breaker, and changes the bearing way of the APS ceramsite (the hollow ceramsite sucks the saturated or nearly saturated ammonium persulfate solution and then carries the solid matter in a vacuum drying way), and matches with a compact brittle resin material as a controlled release thought for coating the capsule coat. Therefore, the contact between the gel breaker and the fracturing fluid during the fracturing process is avoided, the gel breaker breaks in advance, after the fracturing construction is finished, the capsule coat of the brittle resin material is crushed by closing stress, and the particles wrapped in the capsule coat are released to play a gel breaking role. Compared with various existing capsule gel breakers, the novel sustained-release gel breaker prepared by the method has the advantages of strong pressure-bearing capacity, good gel-breaking delaying performance, simple preparation process, economy, applicability and industrial large-scale production.
Drawings
FIG. 1 is an uncoated, vacuum dried breaker microsphere of a solution of drawn ammonium persulfate;
fig. 2 is a coated vacuum dried breaker microsphere of a solution of drawn ammonium persulfate.
Detailed Description
Example 1
A sustained-release guar gum fracturing fluid gel breaker adopts high-strength hollow ceramsite microspheres as a carrier, bears crystals obtained after ammonium persulfate saturated aqueous solution is dried in vacuum, and the surfaces of the hollow ceramsite microspheres are coated with resin and a dispersing agent.
The strength of the high-strength hollow ceramsite microspheres is 30Mpa.
The resin is SR762 type acrylic resin; the dispersing agent is nano calcium carbonate powder.
The preparation method comprises the following specific steps:
(1) Dissolving 25g of ammonium persulfate in 50g of distilled water to obtain an ammonium persulfate aqueous solution;
(2) Adding 165g of hollow ceramsite microspheres into an ammonium persulfate aqueous solution until the hollow ceramsite microspheres are just immersed, and then carrying out vacuum drying at 70 ℃ for 24h for crystallization to obtain 188g of load microspheres;
(3) And adding 2.5g of the mixture containing the resin into 10g of the loaded microspheres, stirring for 5min, adding 10g of nano calcium carbonate, stirring for 5min, standing for 24h, and screening to obtain a finished product A.
In the step (3), the mixture containing the resin is an absolute ethyl alcohol solution containing the resin, wherein 25g of SR762 type acrylic resin and 100g of absolute ethyl alcohol are contained.
Comparative example 1
The preparation method omits the step (3), and the rest is the same as the example 1 to obtain a finished product A'.
Example 2
A sustained-release guar gum fracturing fluid gel breaker adopts high-strength hollow ceramsite microspheres as a carrier, bears crystals obtained after ammonium persulfate saturated aqueous solution is dried in vacuum, and the surfaces of the hollow ceramsite microspheres are coated with resin and a dispersing agent.
The strength of the high-strength hollow ceramsite microspheres is 25Mpa.
The resin is E0578 type acrylic resin; the dispersing agent is nano calcium carbonate powder.
The preparation method comprises the following specific steps:
(1) Dissolving 25g of ammonium persulfate in 65g of distilled water to obtain an ammonium persulfate aqueous solution;
(2) Adding 270g of hollow ceramsite microspheres into an ammonium persulfate aqueous solution until the hollow ceramsite microspheres are just immersed, and then carrying out vacuum drying at 75 ℃ for 24h for crystallization to obtain 290g of loaded microspheres;
(3) And adding 2.0g of the mixture containing the resin into 10g of the loaded microspheres, stirring for 5min, adding 10g of nano calcium carbonate, stirring for 5min, standing for 24h, and screening to obtain a finished product B.
In the step (3), the mixture containing the resin is an absolute ethyl alcohol solution containing the resin, wherein 25g of the E0578 type acrylic resin and 100g of absolute ethyl alcohol are contained.
Comparative example 2
The preparation method omits the step (3), and the rest is the same as the example 2 to obtain a finished product B'.
Example 3
A sustained-release guar gum fracturing fluid gel breaker adopts high-strength hollow ceramsite microspheres as a carrier, bears crystals obtained after ammonium persulfate saturated aqueous solution is dried in vacuum, and the surfaces of the hollow ceramsite microspheres are coated with resin and a dispersing agent.
The strength of the high-strength hollow ceramsite microspheres is 23Mpa.
The resin is epoxy resin; the dispersant is nano calcium carbonate powder.
The preparation method comprises the following specific steps:
(1) Dissolving 25g of ammonium persulfate in 48g of distilled water to obtain an ammonium persulfate aqueous solution;
(2) Adding 165g of hollow ceramsite microspheres into an ammonium persulfate aqueous solution until the hollow ceramsite microspheres are just immersed, and then carrying out vacuum drying at 70 ℃ for 24h for crystallization to obtain 189g of loaded microspheres;
(3) And adding 1.5g of the mixture containing the resin into 10g of the loaded microspheres, stirring for 5min, then adding 10g of nano calcium carbonate, stirring for 5min, standing for 24h, and screening to obtain a finished product C.
In the step (3), the mixture containing the resin is a mixture of the resin and a curing agent, wherein 16.6g of epoxy resin and 4.15g of the curing agent are contained.
Comparative example 3
The preparation method omits the step (3), and the rest is the same as the embodiment 3 to obtain the finished product C'.
Test examples
Weighing 4g of hydroxypropyl guar powder and 4g of organic boron crosslinking agent by using an electronic balance, respectively, weighing 1500g of water in a 2000ml big beaker, adding the hydroxypropyl guar powder while rotating and stirring, and stirring for 5min after completely adding the hydroxypropyl guar powder to fully dissolve the hydroxypropyl guar powder. Then, the weighed organic boron crosslinking agent is added in one step, jelly is formed in about 2min, and the viscosity of the jelly is 19980mPa & s by using a digital display viscosity meter.
Respectively taking a finished product A, B, C and finished products A ', B ' and C ' (equivalent to the step (1) that 1g of ammonium persulfate is adopted), respectively adding the finished products into 150g of jelly, placing the jelly into a 70 ℃ thermostat to record viscosity change within 2h, respectively taking out and mashing a finished product A, B, C (simulating a closed stress crushing release mechanism after fracturing operation is finished), adding the crushed product into new jelly, and recording the viscosity change of the jelly within 2h in the 70 ℃ thermostat again:
TABLE 1
Comparing the data in the table 1, the invention has good delayed release performance compared with uncoated gel breaker microspheres, within the first 30min, the loss of sand carrying capacity caused by premature hydration gel breaking due to contact between the fracturing fluid gel and the gel breaker can be basically avoided, the viscosity of the gel can be still kept at 1000 mPa & s within 60min, and after the gel is smashed and released, the viscosity of the fracturing fluid gel can be rapidly reduced.
Claims (8)
1. The sustained-release type guar gum fracturing fluid gel breaker is characterized by comprising a loaded microsphere and a mixture containing a brittle resin material; the load microsphere adopts a hollow ceramsite microsphere as a carrier, and bears the crystal obtained after vacuum drying of the ammonium persulfate aqueous solution; the surface of the load microsphere is coated with a mixture containing a brittle resin material and a dispersant; the brittle resin material is epoxy resin or SR762 type acrylic resin or E0578 type acrylic resin or a mixture thereof;
the strength of the hollow ceramsite microspheres is 23-30Mpa;
the dispersing agent is nano calcium carbonate powder;
in the ammonium persulfate aqueous solution, the mass of ammonium persulfate is 27-35% of that of distilled water;
the mass ratio of the hollow ceramsite microspheres to the ammonium persulfate aqueous solution is (2.2): 1 to 3:1;
the dosage of the mixture containing the brittle resin material is 15 to 25 percent of the mass of the loaded microsphere.
2. The preparation method of the sustained-release guar gum fracturing fluid gel breaker of claim 1, which is characterized by comprising the following specific steps:
(1) Dissolving ammonium persulfate in distilled water to obtain an ammonium persulfate aqueous solution;
(2) Adding hollow ceramsite microspheres into an ammonium persulfate aqueous solution until the hollow ceramsite microspheres are just immersed, and then drying in vacuum and crystallizing to obtain loaded microspheres; the vacuum drying temperature is 70-75 ℃, and the drying time is 24h;
(3) And adding a mixture containing a brittle resin material into the loaded microspheres, stirring, adding a dispersing agent, stirring, standing, and screening to obtain a finished product.
3. The preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, wherein in the step (1), the mass of the ammonium persulfate is 27-35% of the mass of the distilled water.
4. The preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, wherein in the step (2), the mass ratio of the hollow ceramsite microspheres to the ammonium persulfate aqueous solution is 2.2:1 to 3:1.
5. the preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, characterized in that in the step (3), the amount of the mixture containing the brittle resin material is 15-25% of the mass of the loaded microspheres.
6. The preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, wherein in the step (3), the mixture containing the brittle resin material is a mixture of resin and absolute ethyl alcohol, and the mass ratio of the resin: absolute ethanol =1:4.
7. the preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, wherein in the step (3), the mixture containing the brittle resin material is a mixture of a resin and a curing agent, and the mass ratio of the resin: curing agent =4:1.
8. the preparation method of the sustained-release guar gum fracturing fluid gel breaker according to claim 2, wherein in the step (3), the mixing time is 5min, the stirring time is 5min, and the standing time is 24h.
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| CN102108293A (en) * | 2009-12-23 | 2011-06-29 | 中国石油天然气股份有限公司 | Preparation method of chemical temporary plugging rubber plug slow-release gel breaker |
| CN102690645B (en) * | 2012-06-08 | 2014-07-02 | 中国海洋石油总公司 | Sustained-release gel-breaking type fracturing propping agent and preparation method thereof |
| CN106566522B (en) * | 2016-11-14 | 2019-06-25 | 常熟理工学院 | A kind of timing rupture release type microcapsule degelling agent and preparation method thereof |
| CN111778011A (en) * | 2020-06-29 | 2020-10-16 | 中国石油天然气股份有限公司 | Coated propping agent with sustained-release gel breaking effect and preparation method thereof |
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