CN112646564B - Magnetic hydrophobic propping agent and preparation method thereof - Google Patents
Magnetic hydrophobic propping agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnetic hydrophobic propping agent and a preparation method thereof. Blending the propping agent aggregate with the liquid hydrophobic resin glue solution containing the magnetic powder, and then curing to obtain the magnetic powder. The invention adopts the hydrophobic resin glue solution containing magnetic powder to coat the modified propping agent aggregate, has strong universality, is suitable for various conventional propping agents such as raw sand, ceramsite and the like, is suitable for the preparation of the ton-level propping agent, and is simple and easy to operate. Not only the density of the magnetic hydrophobic propping agent is reduced, but also the preparation cost is greatly reduced.
Description
Technical Field
The invention relates to a magnetic hydrophobic propping agent and a preparation method thereof, belonging to the technical field of hydraulic fracturing in petroleum and natural gas exploitation processes.
Background
Hydraulic fracturing is an important technical means for improving the yield of an oil and gas well, and is used for achieving a key yield increasing effect on shale and tight sandstone reservoirs of conventional low-permeability and ultra-low-permeability oil and gas reservoirs or unconventional oil and gas reservoirs, particularly unconventional reservoirs, and underground oil and gas is difficult to extract without hydraulic fracturing. Hydraulic fracturing is to pump a fracturing fluid into a stratum by using a high-pressure pump set, so that one or more cracks with a certain geometric dimension are formed in the stratum, the lengths of the cracks are generally from tens of meters to hundreds of meters, the heights are from tens of meters to tens of meters, and the widths are several millimeters wide. Then the sand-carrying fluid with proppants (a mixture of fracturing fluid and proppants) is injected into the fracture. After the fracturing is finished, the fracturing fluid breaks gel and is discharged back to the ground, the propping agent is left in the cracks to play a role in supporting the cracks, the cracks are kept in an open state, and the pores among propping agent particles provide a circulation channel for oil, gas and water of the stratum, so that the fracturing yield increasing effect is achieved. Propping agent is one of the key factors of good yield increasing effect, and good propping agent has higher flow conductivity (width of crack multiplied by permeability of crack) and can provide smooth flow channels for oil, gas and water.
The traditional propping agent mainly comprises three major categories of natural sand, resin coated sand and ceramsite, and generally, the strength and the flow conductivity are sequentially enhanced. According to the formation characteristics, depth characteristics and the like of the fracturing region, different types of proppants are selected, and mainly comprise: natural quartz sand, artificial haydite, glass bead, walnut shell, high molecular synthetic microsphere, etc. After the propping agent is pumped into the stratum, adverse factors such as backflow, embedding, dissolution, crushing and the like can occur, and the propping agent has no selectivity to oil water. Fracturing of an oil and gas well requires proppants ranging from tens to hundreds of tons, and fracturing of unconventional reservoirs such as shale often requires from thousands to tens of thousands of tons of proppants.
The purpose of oil well fracturing is to increase the production of oil, and to reduce the production of water as much as possible. However, the conventional fracturing propping agent has no effect of controlling water and increasing oil, so that the water content of some oil wells is too high after fracturing, the development result is high, and the yield increasing effect is not ideal.
Chinese patent document CN 106546658A discloses a device for measuring proppant distribution in a rock formation and a measuring method thereof. The specific process for making the magnetic proppants is mentioned therein as: selecting a plurality of small iron particles and magnetizing the small iron particles; screening and selecting a qualified product; the oil shale slag, bauxite, manganese mineral powder, iron powder and binder are mixed according to a certain proportion and then attached to the outer surface of the small iron particles, and a layer of resin is uniformly coated on the outermost layer of the small iron particles to prepare the propping agent. Therefore, the main solid material of the magnetic propping agent is iron material, and has higher density and higher cost than the traditional sand and ceramsite.
The Chinese patent document CN105670600A discloses a water acid-sensitive deformation magnetic tracing function self-suspension propping agent and a preparation method thereof, wherein a magnetic additive used by the magnetic propping agent is a magnetic rare earth material, and has the advantages of high cost, less addition amount, low magnetic intensity and main key performance of the self-suspension function generated by coating a water bloom layer.
Chinese patent document CN109423271a discloses a bulk-expanded magnetic self-suspending proppant and a method for preparing the same; chinese patent document CN109423270a discloses a tackified magnetic self-suspending proppant useful for crack monitoring and a method for preparing the same. The aggregate of the magnetic propping agent used in the two methods is Fe 3 O 4 、γ-Fe 2 O 3 、CoFe 2 O 4 、MnFe 2 O 4 And NiFe 2 O 4 At least one of the materials is also higher in density and higher in cost than the traditional sand and ceramsite.
In a word, the application of the magnetic propping agent in the fracturing process is studied at present, but the defects of high preparation or modification cost, high magnetic material density, complex preparation process and the like exist.
Therefore, the development of the high-magnetic propping agent which is simple and convenient to operate, simple in process flow and high in universality is necessary, and meanwhile, the cost is reduced, and the degree of harm to human bodies and the environment is reduced.
Disclosure of Invention
Aiming at the defects of the prior art, particularly the defects of high density and high cost caused by the fact that the existing magnetic propping agent takes magnetic substances as aggregate, the invention provides a magnetic hydrophobic propping agent and a preparation method thereof. The proppant disclosed by the invention has the advantages that the procedure of adding other chemical additives is not needed except the magnetic hydrophobic glue solution, the improved proppant has good stronger magnetic property, the proppant is suitable for various proppants such as raw sand, ceramsite and the like, and the complexity of chemical reaction and operation implementation in the traditional modification process is reduced. The method is high in universality, suitable for propping agents of different sizes and different types, capable of reducing the cost of hydrophobic modification of the propping agents, and suitable for large-scale industrial application.
The invention is realized by the following technical scheme:
a magnetic hydrophobic propping agent comprises propping agent aggregate, wherein the surface of the propping agent aggregate is coated with magnetic hydrophobic resin, and the magnetic hydrophobic resin comprises a magnetic material and hydrophobic resin.
According to the invention, preferably, the propping agent aggregate is a common propping agent such as quartz sand or ceramic particles or a plurality of propping agents such as walnut shells and glass spheres. Preferably, the particle size of the propping agent aggregate is 20-140 meshes. The invention can adopt the conventional propping agent as the aggregate, has wide applicability, small density and low cost, and is very favorable for large-scale popularization and application.
According to the invention, preferably, the magnetic material is magnetic powder, is hard magnetic single domain particles, and can be purchased in the market. The magnetic powder may be obtained by magnetizing iron powder. The particle size of the magnetic powder is in the range of 100 nanometers to 5 micrometers.
According to the present invention, the hydrophobic resin is preferably a fluorinated acrylic resin, a fluorinated dopamine resin, a dopamine resin, an acrylate resin, a silicone resin, a polyurethane resin, an epoxy resin, or other resins having similar properties, etc. The hydrophobic resin is selected, so that not only can the magnetic propping agent endow a hydrophobic function, but also the strength of the propping agent can be increased, the propping agent can be prevented from being embedded, the dissolution degree of the propping agent under the high-temperature and high-pressure condition of the stratum can be reduced, and the migration of broken propping agent fragments can be prevented.
According to the invention, preferably, the mass ratio of the magnetic powder to the hydrophobic resin in the magnetic hydrophobic resin is 100: (60-90), further preferably 100: (70-80).
According to the invention, preferably, the mass ratio of the proppant aggregate to the magnetic hydrophobic resin is 100: (10-50), further preferably 100: (20-40). The magnetic material has too small specific gravity, which leads to poor coating degree, uneven coating and bare ceramsite; the excessive specific gravity of the magnetic material can cause the separation of the redundant magnetic material and the propping agent material, and the improvement degree of the haydite bare phenomenon is small.
According to the invention, the preparation method of the magnetic hydrophobic propping agent comprises the following steps:
blending the propping agent aggregate with the liquid hydrophobic resin glue solution containing the magnetic powder, and then curing to obtain the magnetic powder.
According to the invention, preferably, the curing mode is to preheat the used propping agent aggregate or add liquid hydrophobic resin glue solution and then heat the mixture to cure the liquid hydrophobic resin glue solution;
further preferably, the proppant aggregate is mixed with the liquid hydrophobic resin glue solution containing magnetic powder and then heated to 30-90 ℃ under stirring for 0.2-6 hours for curing.
According to a preferred embodiment of the method for preparing a magnetic hydrophobic proppant of the present invention, it comprises the steps of:
(1) Cleaning the propping agent aggregate with water or acid liquor or alkali liquor for 0.5-3 hours to obtain cleaned propping agent aggregate;
(2) Adding magnetic powder into the liquid hydrophobic resin glue solution, and uniformly mixing to obtain the magnetic hydrophobic resin glue solution;
(3) Adding the magnetic hydrophobic resin glue solution into the cleaned proppant aggregate, and uniformly stirring for 5-60 minutes to blend the proppant aggregate and the magnetic hydrophobic resin glue solution to obtain a blend;
(4) And heating the blend to 30-90 ℃ under stirring for 0.2-6 hours, and curing to obtain the magnetic hydrophobic modified propping agent.
The liquid hydrophobic resin glue solution used in the invention is a conventional hydrophobic glue solution, can be purchased or prepared in a laboratory, such as acrylic acid, acrylic acid esters, dopamine, epoxy, polyurethane, organosilicon hydrophobic glue solution and the like, and selects the hydrophobic time according to the types of the glue solution and the difference of the hydrophobic effect. The raw materials and equipment used in the invention are all the prior art unless otherwise specified.
The beneficial effects of the invention are as follows:
1. the invention adopts the hydrophobic resin glue solution containing magnetic powder to coat the modified propping agent aggregate, has strong universality, is suitable for various conventional propping agents such as raw sand, ceramsite and the like, is suitable for the preparation of the ton-level propping agent, and is simple and easy to operate. Not only the density of the magnetic hydrophobic propping agent is reduced, but also the preparation cost is greatly reduced.
2. The hydrophobic resin glue solution used in the invention is a conventional hydrophobic glue solution, the sources of raw materials are wide and easy to obtain, and the modified magnetic hydrophobic propping agent has good magnetism and surface hydrophobicity through test, is beneficial to use in high-speed channel fracturing and is beneficial to exploitation of oil gas.
3. The invention carries out surface treatment on the existing propping agent to realize new functions of magnetism and hydrophobicity, and can increase the strength of the propping agent, prevent the propping agent from being embedded, reduce the dissolution degree of the propping agent under the high-temperature and high-pressure condition of the stratum and prevent the migration of broken propping agent fragments. The method does not need to change the components and the production process of the propping agent, and has the characteristics of simple operation, low cost, short production time, suitability for large-scale industrialized application and the like.
Drawings
FIG. 1 is a diagram of a magnetic hydrophobically modified ceramsite product made in accordance with example 2;
FIG. 2 is a drawing showing the magnetic attraction of the magnetic hydrophobically modified ceramsite prepared in example 2;
FIG. 3 is a diagram of the magnetic hydrophobically modified ceramsite product of comparative example 2.
Detailed Description
The invention is further illustrated by, but not limited to, the following specific examples.
Example 1
The magnetic hydrophobic modified propping agent is prepared by adding magnetic hydrophobic resin glue solution into propping agent aggregate, uniformly stirring to enable the magnetic hydrophobic glue solution to wet the surface of the propping agent, and then solidifying.
The preparation method comprises the following steps:
(1) The liquid hydrophobic acrylic resin pre-cured glue solution prepared by the prior art can be referred to Feng Runjiang. Synthesis of the hydrophobic modified acrylic emulsion thickener and its rheological behavior [ D ]. University of North China's university of technology, 2011.
(2) Cleaning quartz sand with different particle sizes by using water, acid liquor or alkali liquor for 2 hours to obtain cleaned quartz sand;
(3) Adding 80% of magnetic powder by mass into the liquid hydrophobic acrylic resin glue solution, and uniformly mixing to prepare the liquid magnetic resin glue solution; the magnetic powder is hard magnetic single domain particles, and can be purchased in the market;
(4) Taking 50 parts of liquid magnetic hydrophobic acrylic resin glue solution, 100 parts of cleaned quartz sand, adding the magnetic hydrophobic acrylic resin glue solution into the cleaned quartz sand, and stirring to uniformly mix the quartz sand and the magnetic hydrophobic acrylic resin glue solution, thereby achieving the effect that the surface of the quartz sand is coated by the magnetic hydrophobic acrylic resin glue solution; and then heating to 60 ℃, discharging after 2 hours, and cooling to obtain the magnetic hydrophobic modified propping agent.
Example 2
The magnetic hydrophobic modified propping agent is prepared by adding hydrophobic dopamine resin glue solution containing magnetized iron powder into propping agent aggregate, uniformly stirring, coating the surface of propping agent aggregate with the hydrophobic dopamine resin glue solution containing magnetized iron powder particles, and then solidifying.
The preparation method comprises the following steps:
(1) The hydrophobic dopamine resin glue is prepared by the prior art, and reference is made to Wang X L, ye Q A, liu J X, et al, low surface energy surfaces from self-assembly of perfluoropolymer with sticky functional groups [ J ]. Journal of Colloid and Interface Science,2010,351 (1): 261-266.
(2) Washing the ceramsite with water, acid liquor or alkali liquor for 2 hours to obtain washed ceramsite;
(3) Adding 70% of magnetized iron powder into the liquid hydrophobic dopamine resin glue solution, and uniformly mixing to prepare liquid magnetic dopamine resin glue solution;
(4) Taking 45 parts of magnetic hydrophobic dopamine resin glue solution, cleaning 100 parts of ceramsite, adding the magnetic hydrophobic dopamine resin glue solution into the cleaned ceramsite, and uniformly stirring for 30 minutes to uniformly mix the ceramsite and the magnetic hydrophobic dopamine resin glue solution; and then heating to 60 ℃, discharging after 2 hours, and cooling to obtain the magnetic hydrophobic modified propping agent.
The photograph of the magnetic hydrophobically modified proppant obtained in this example is shown in fig. 1, and the photograph of the magnetic adsorption effect is shown in fig. 2. As can be seen from fig. 1 and 2, the magnetic hydrophobic modified propping agent disclosed by the invention has uniform surface coating and stronger magnetism.
Example 3
The magnetic hydrophobic modified propping agent is prepared by adding magnetic hydrophobic resin glue solution into propping agent aggregate, uniformly stirring to enable the magnetic hydrophobic glue solution to wet the surface of the propping agent, and then solidifying.
The preparation method comprises the following steps:
(1) The liquid hydrophobic fluorinated acrylic resin glue solution prepared by the prior art can be referred to Wuyang soft matter interface friction drag reduction regulation and control research [ D ]. The institute of chemistry and physics of Orchis, china academy of sciences, 2015.
(2) Cleaning glass spheres with different particle sizes by using water, acid liquor or alkali liquor for 2 hours to obtain cleaned glass spheres;
(3) Adding 60% of magnetic powder by mass into the liquid hydrophobic fluorinated acrylic resin glue solution, and uniformly mixing to prepare the liquid magnetic resin glue solution; the magnetic powder is hard magnetic single domain particles, and can be purchased in the market;
(4) Taking 20 parts of liquid magnetic hydrophobic fluorinated acrylic resin glue solution, 100 parts of cleaned glass spheres, adding the magnetic hydrophobic fluorinated acrylic resin glue solution into the cleaned glass spheres, and stirring to uniformly mix the glass spheres with the magnetic hydrophobic fluorinated acrylic resin glue solution so as to achieve the effect that the surfaces of the glass spheres are coated by the magnetic hydrophobic fluorinated acrylic resin glue solution; and then heating to 40 ℃, discharging after 5 hours, and cooling to obtain the magnetic hydrophobic modified propping agent.
Example 4
A magnetic hydrophobic modified propping agent is prepared through adding the hydrophobic polyurethane resin adhesive containing magnetized iron powder to the propping agent aggregate, uniformly stirring to make the hydrophobic polyurethane resin adhesive containing magnetized iron powder particles coat the surface of propping agent aggregate, and solidifying.
The preparation method comprises the following steps:
(1) The hydrophobic polyurethane resin glue solution is prepared by adopting the prior art, and reference can be made to Mo Hao, the preparation of vinyl acrylic polyurethane hydrophobic anticorrosive paint and performance research [ D ], harbin university of industry, 2011.
(2) Washing the ceramsite with water, acid liquor or alkali liquor for 2 hours to obtain washed ceramsite;
(3) Adding 85% of magnetized iron powder into the liquid hydrophobic polyurethane resin glue solution, and uniformly mixing to prepare liquid magnetic dopamine resin glue solution;
(4) Taking 30 parts of magnetic hydrophobic dopamine resin glue solution, cleaning 100 parts of ceramsite, adding the magnetic hydrophobic polyurethane resin glue solution into the cleaned ceramsite, and uniformly stirring for 30 minutes to uniformly mix the ceramsite and the magnetic hydrophobic polyurethane resin glue solution; and then heating to 70 ℃, discharging after 1 hour, and cooling to obtain the magnetic hydrophobic modified propping agent.
Comparative example 1
As described in example 2, the difference is that:
and directly adding magnetized iron powder into the hydrophobic dopamine resin glue solution, uniformly mixing, and curing to obtain the magnetic hydrophobic modified propping agent.
Comparative example 2
As described in example 2, the difference is that:
taking 70 parts of magnetic hydrophobic dopamine resin glue solution, 100 parts of cleaned ceramsite, and uniformly mixing.
The effect is shown in figure 3.
As can be seen from fig. 3, the magnetic hydrophobic dopamine resin glue solution is too high, so that the ceramsite cannot be completely coated, and a large amount of agglomeration occurs.
Test example 1
The proppant obtained in example 2 and comparative example 1 were tested for density and suspension in aqueous solution, and the results are shown in table 1.
TABLE 1
| Index (I) | Example 2 | Comparative example 1 |
| Density g/cm 3 | 1.8 | 6.9 |
| Suspension in aqueous solution | Floating | Precipitation |
As can be seen from table 1, the proppant obtained by directly coating the magnetized iron powder with the resin dope of comparative example 1 was so dense that it precipitated in an aqueous solution. The magnetic hydrophobically modified proppant obtained in example 2, however, not only has a greatly reduced density compared to comparative example 1, but also floats in aqueous solution. Is very beneficial to the application in high-speed channel fracturing.
Claims (5)
1. The magnetic hydrophobic propping agent comprises propping agent aggregate, and is characterized in that the surface of the propping agent aggregate is coated with magnetic hydrophobic resin, and the magnetic hydrophobic resin comprises a magnetic material and hydrophobic resin;
the mass ratio of the magnetic powder to the hydrophobic resin in the magnetic hydrophobic resin is 100: (60-90), wherein the mass ratio of the proppant aggregate to the magnetic hydrophobic resin is 100: (10-50);
the particle size of the propping agent aggregate is 20-140 meshes;
the magnetic material is magnetic powder, and the particle size range of the magnetic powder is 100 nanometers-5 microns;
the hydrophobic resin is fluorinated acrylic resin, fluorinated dopamine resin, acrylic resin, organic silicon resin, polyurethane resin or epoxy resin.
2. The magnetic hydrophobic proppant of claim 1, wherein the proppant aggregate is quartz sand, ceramic particles, walnut shells, or glass spheres.
3. A method of preparing the magnetic hydrophobic proppant of claim 1, comprising the steps of:
blending the propping agent aggregate with the liquid hydrophobic resin glue solution containing the magnetic powder, and then curing to obtain the magnetic powder.
4. A method of preparing a magnetic hydrophobic proppant as set forth in claim 3 wherein the curing is by preheating the proppant aggregate used or adding a liquid hydrophobic resin cement followed by heating to cure the liquid hydrophobic resin cement.
5. The method of preparing a magnetic hydrophobic proppant according to claim 4, wherein the proppant aggregate is mixed with a liquid hydrophobic resin glue solution containing magnetic powder, and then heated to 30-90 ℃ under stirring for 0.2-6 hours, and cured.
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| CN105670600A (en) * | 2016-03-07 | 2016-06-15 | 王展旭 | Water acid-sensitivity deformation magnetic tracer function self-suspension propping agent and preparation method thereof |
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| US7754659B2 (en) * | 2007-05-15 | 2010-07-13 | Georgia-Pacific Chemicals Llc | Reducing flow-back in well treating materials |
| CN106883837A (en) * | 2017-02-17 | 2017-06-23 | 北京大学 | A kind of hydrophobically modified proppant and preparation method thereof |
| CN109423270A (en) * | 2017-09-01 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of increasing stick type magnetism of beneficial Crack Monitoring is from suspended prop and preparation method thereof |
| CN110157405B (en) * | 2019-04-23 | 2020-11-10 | 中国石油大学(北京) | Tectorial membrane proppant for unconventional reservoir hydraulic fracturing, preparation and application |
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