CN112745819A - Degradable temporary plugging agent and preparation method thereof - Google Patents

Degradable temporary plugging agent and preparation method thereof Download PDF

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Publication number
CN112745819A
CN112745819A CN202110159979.7A CN202110159979A CN112745819A CN 112745819 A CN112745819 A CN 112745819A CN 202110159979 A CN202110159979 A CN 202110159979A CN 112745819 A CN112745819 A CN 112745819A
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plugging agent
temporary plugging
polyester material
degradable
polyglycolide
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CN112745819B (en
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郑存川
张太亮
黄朵
付玉龙
唐晓莉
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Sichuan Kuineng Environmental Protection Technology Co ltd
Southwest Petroleum University
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Sichuan Kuineng Environmental Protection Technology Co ltd
Southwest Petroleum University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
    • C09K8/504Compositions based on water or polar solvents
    • C09K8/506Compositions based on water or polar solvents containing organic compounds
    • C09K8/508Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/5086Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

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  • General Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a degradable temporary plugging agent and a preparation method and application thereof, relating to the technical field of oil and gas development; the temporary plugging agent comprises a polyester material and inorganic nanoparticles added in the polyester material, wherein the addition amount of the inorganic nanoparticles in the polyester material is 1-5%. The invention also discloses a preparation method of the degradable temporary plugging agent, which is to melt, blend and mold the polyester material and the inorganic nano-particles to obtain temporary plugging agent particles with the particle size of 286.3-525.7 microns. The degradable temporary plugging agent disclosed by the invention is prepared by dispersing inorganic nanoparticles into a polyester material, so that the temporary plugging agent which is strong in plugging capability, rapid in plugging removal and free from environmental pollution is formed.

Description

Degradable temporary plugging agent and preparation method thereof
Technical Field
The invention belongs to the technical field of oil and gas development, and particularly relates to a degradable temporary plugging agent and a preparation method thereof.
Background
After the water injection oil well enters the middle and later stages of development, the comprehensive water content of the oil field rises, a part of main oil layers are completely flooded, and relatively low-permeability oil layers with higher oil saturation cannot be used, so that the development difficulty of the oil field is increased, and the comprehensive water content rises rapidly. In order to reduce the water content of the oil well and provide recovery from the oil field, the prior art generally adopts two methods of selectively plugging a high permeability zone and directing a development destination layer to a low permeability layer to increase the oil production.
In the well killing, well washing, acidizing and well drilling processes, because the bottom layer has heterogeneity, the treatment fluid preferentially enters a high permeable layer or a large crack with relatively small resistance, so that the oil layer is greatly damaged. Therefore, temporary plugging by using a temporary plugging agent is needed before operation and construction, so that the leakage of working fluid can be effectively reduced, and the effect of protecting an oil-gas reservoir is achieved. The jelly formed by the temporary plugging agent has strong plugging capability, so that other working fluids cannot enter the stratum, and the purpose of temporary plugging is achieved. After the operation is finished, the gel breaks and scratches water, and the blockage is automatically removed, so that the oil well recovers the capacity, and the purpose of protecting the oil-gas layer is achieved.
The temporary plugging agent has the characteristics of plugging and plugging removal materials. Firstly, the gel strength is required to be achieved during plugging, sandstone and stratum with different pores are required to be plugged in a relatively short time, and the gel needs to be rapidly expanded underground to fill the pores so as to plug liquid flow; after plugging, the material is gradually degraded to slowly become flowable liquid, the pores of the stratum can be recovered under the action of pressure, and neither the material gel nor the material liquefy the stratum is polluted, so that the development of a proper temporary plugging agent has important significance for the recovery ratio of the oil field.
Disclosure of Invention
The invention provides a degradable temporary plugging agent aiming at the problems that the plugging capability of the conventional temporary plugging agent is strong, the deblocking speed cannot be achieved simultaneously, and the environmental pollution is serious.
The invention also discloses a preparation method of the degradable temporary plugging agent, which is simple and easy to popularize and use.
The specific technical scheme of the invention is as follows: the degradable temporary plugging agent comprises a polyester material and inorganic nanoparticles added in the polyester material, wherein the addition amount of the inorganic nanoparticles in the polyester material is 1-5%.
In the technical scheme, the inorganic nanoparticles are added into the polyester material through melting and blending and are used as a dispersed phase and a catalyst in the copolymerization process of the polyester material to form the degradable copolyester inorganic nanoparticle composite temporary plugging agent, wherein the selected polyester material has good degradability, and the nanoparticles with good reinforcing property and strong environmental friendliness are selected, so that the composite temporary plugging agent can better cope with the conditions of complex strata.
Further, the polyester material is at least two of polylactic acid ester, polyglycolide and polybutylene succinate. The molecular weight of the polylactic acid ester adopted in the polyester material is 40000-65000; the molecular weight of the polyglycolide is 2500-5000; the molecular weight of the poly (butylene succinate) is 28600-75500.
The polyester material is polylactic acid ester with the mass ratio of 5-7: 1-3, is a novel environment-friendly material, has good biodegradability, biocompatibility and absorbability, and can be recycled from raw materials to wastes; polyglycolide has no toxicity and good biocompatibility, the intermediate product of hydrolysis is glycolic acid, and the final products are carbon dioxide and water which meet the requirement of environmental protection; the poly (butylene succinate) is a novel aliphatic biodegradable polyester material, has low price, good physical and mechanical properties, easy processing and forming and the like. Preferably, the mass ratio of the polylactic acid ester to the polyglycolide to the polybutylene succinate is as follows: 3:1:1, and the polyester material obtained in the proportion has the best water absorption swelling performance which can reach 39 times.
Further, the inorganic nano-particles are at least one of nano-silicon dioxide, nano-titanium dioxide and nano-zirconium dioxide, preferably nano-titanium dioxide, and have good dispersibility and weather resistance and no biotoxicity. .
Further, the particle size of the inorganic nano-particles is 27nm to 143 nm.
The invention also discloses a preparation method of the degradable temporary plugging agent, which is mainly to melt, blend and form the polyester material and the inorganic nano-particles to obtain temporary plugging agent particles with the particle size of 286.3-525.7 microns.
The preparation method specifically comprises the following steps:
s1: preparation of polyester Material
Selecting at least two of polylactic acid ester, polyglycolide and polybutylene succinate, and mixing uniformly in advance according to a formula;
s2: melting and blending the polyester material and the inorganic nano particles;
s3: the polyester material was processed to melt using a two-roll mixer and the nanoparticles were sprinkled evenly between the two rolls during melting.
S4: and forming the cooled temporary plugging agent by using a ball mill.
Further, the S2 specifically includes the following steps:
s21: and opening the double-roller mixing mill, setting the rotating speed to be 10-25 r/min, setting the temperature, and placing the polyester material on a double roller after the set temperature is reached.
S22: the nanoparticles prepared in advance were slowly and uniformly sprinkled between the twin rolls in the molten state of the polyester material.
Further, in the step S22, the polyester material is processed by a two-roll mixing mill and is open-milled for 0.5 to 2.5 hours at the temperature of 180 to 240 ℃, and after the nano particles are uniformly sprinkled between two rolls, the polyester material is cooled;
further, in S3: and (4) setting the rotating speed of a ball milling barrel to be 200-500 r/min by using a ball mill to ball mill and form the cooled temporary plugging agent.
Further, in the S3, the temporary plugging agent is shaped into particles of 286.3 μm to 525.7 μm by ball mill pulverization after cooling.
The invention provides a degradable temporary plugging agent which has strong plugging capability, quick unblocking and serious environmental pollution, and is dispersed into a polyester material by adopting inorganic nano particles through a melt blending method.
The degradable temporary plugging agent disclosed by the invention adopts at least two polyester materials to form a copolymer, and the polylactic acid ester is a novel environment-friendly material, has good biodegradability, biocompatibility and absorbability, and can be recycled from raw materials to wastes; polyglycolide has no toxicity and good biocompatibility, the intermediate product of hydrolysis is glycolic acid, and the final products are carbon dioxide and water which meet the requirement of environmental protection; the poly (butylene succinate) is a novel aliphatic biodegradable polyester material, has low price, good physical and mechanical properties, easy processing and forming and the like.
The invention also discloses a method for preparing the degradable temporary plugging agent by melt blending, no solvent or additive is added, compared with the traditional solvent method, the method has the advantages of simple process and short processing time, and the prepared reagent can be directly used in engineering.
The viscosity of the degradable temporary plugging agent disclosed by the invention can reach 79 mPa.s, the expansion multiple can reach 32 times, the temporary plugging strength can reach 7.9kPa, and the degradation rate can reach 98.3% at the temperature of 100 ℃.
Detailed Description
Example 1
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: 70% of polylactic acid ester, 29% of polyglycolide and 1% of nano silicon dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was switched on, the temperature set at 240 ℃ and, after reaching the set temperature, the polyester material was open-milled on two rolls at 15 r/min.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after mixing for 1.5h, and cooling;
s3: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 300r/min and using a ball mill, and the particle size D50 is as follows: 347.5 μm.
Example 2
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: 68% of polylactic acid ester, 27% of polyglycolide and 5% of nano silicon dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was turned on, the temperature set at 240 ℃ and, after reaching the set temperature, the polyester material was scoured on two rolls for 1.5h at 15 r/min.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after mixing for 1.5h, and cooling;
s3: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 300r/min and using a ball mill, and the particle size D50 is as follows: 342.7 μm.
Example 3
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: 65% of polylactic acid ester, 32% of polyglycolide and 3% of nano silicon dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was turned on, the temperature set at 240 ℃ and, after reaching the set temperature, the polyester material was scoured on two rolls for 1.5h at 15 r/min.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after mixing for 1.5h, and cooling;
s3: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 300r/min and using a ball mill, and the particle size D50 is as follows: 328.1 μm.
Example 4
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: the formula comprises the following components in percentage by mass: 57.6 percent of polylactic acid ester, 19.2 percent of polyglycolide, 19.2 percent of polybutylene succinate, 2 percent of nano silicon dioxide and 2 percent of nano titanium dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was turned on, the temperature set at 180 ℃ was reached, and after the set temperature was reached, the polyester material was scoured on the two rolls at 10r/min for 0.5 h.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after 0.5h of mixing, and cooling; s3: the polyester material was processed to melt using a two-roll mixer and the nanoparticles were sprinkled evenly between the two rolls during melting.
S3: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 200r/min and using a ball mill, and the particle size D50 is as follows: 525.7 μm.
Example 5
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: the formula comprises the following components in percentage by mass: 57.6 percent of polylactic acid ester, 19.2 percent of polyglycolide, 19.2 percent of polybutylene succinate, 2 percent of nano silicon dioxide and 2 percent of nano titanium dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was turned on, the temperature set at 240 ℃ was reached, and after the set temperature was reached, the polyester material was slit on the two rolls at 25r/min for 2.5 h.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after 2.5h of mixing, and cooling;
s4: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 500r/min and using a ball mill, and the particle size D50 is as follows: 286.3 μm.
Example 6
The present embodiment prepares a degradable temporary plugging agent, and the formula thereof comprises the following components by mass: the formula comprises the following components in percentage by mass: 57.6 percent of polylactic acid ester, 19.2 percent of polyglycolide, 19.2 percent of polybutylene succinate, 2 percent of nano silicon dioxide and 2 percent of nano titanium dioxide.
The specific preparation method comprises the following steps:
s1: preparation of polyester Material
Weighing polylactic acid ester and polyglycolide according to the formula, and mixing uniformly in advance according to the formula.
S21: the two-roll mixer was turned on, the temperature set at 220 ℃ and, after reaching the set temperature, the polyester material was slit on the two rolls at 20r/min for 2 h.
S22: slowly and uniformly sprinkling the prepared nano particles between two rollers in a molten state of the polyester material; stopping mixing after mixing for 2h, and cooling;
s3: after cooling, the temporary plugging agent is crushed into temporary plugging agent powder A by setting the rotating speed of a ball milling tank to be 350r/min and using a ball mill, and the particle size D50 is as follows: 315.9 μm.
Comparative example 1
The polyester material was selected only from polylactic acid ester, and the amounts of other components added and the production method were substantially the same as in example 6, to obtain comparative sample 1.
Comparative example 2
Comparative sample 2 was obtained according to the formulation in example 6, using nanosilica as nanoparticles.
Respectively measuring the viscosity at 80 ℃ of products A to F obtained in examples 1 to 6 and comparative examples 1 to 2 and comparative samples 1 to 2; and measuring the expansion times and the compressive strengths of the products A to F and the comparison samples 1 to 2 and the final degradation rate at 100 ℃ at room temperature; the test results are as follows:
Figure BDA0002936117380000061
from the evaluation results, the viscosity of the temporary plugging agent prepared by the application document can reach 1248.6 mPa.S, the expansion multiple can reach 38 times, the temporary plugging strength can reach 33MPa, the degradation rate at 100 ℃ can reach 99.3%, the plugging capability is strong, the plugging removal is rapid, and the polyester material can be decomposed into small molecular compounds which can be absorbed by the environment after the plugging removal, so that the environment is not polluted.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (9)

1. The degradable temporary plugging agent is characterized by comprising a polyester material and inorganic nanoparticles added in the polyester material, wherein the addition amount of the inorganic nanoparticles in the polyester material is 1-5%.
2. The degradable temporary plugging agent according to claim 1, wherein said polyester material is at least two of polylactic acid ester, polyglycolide and polybutylene succinate.
3. The degradable temporary plugging agent according to claim 2, wherein the polyester material is polylactic acid ester, polyglycolide and polybutylene succinate in a mass ratio of 5-7: 1-3.
4. The degradable temporary plugging agent according to claim 3, wherein the molecular weight of the polylactic acid ester is 40000-65000; the molecular weight of the polyglycolide is 2500-5000; the molecular weight of the poly (butylene succinate) is 28600-75500.
5. The degradable temporary plugging agent according to claim 1, wherein the inorganic nanoparticles are at least one of nano silicon dioxide, nano titanium dioxide and nano zirconium dioxide.
6. The degradable temporary plugging agent of claim 5, wherein said inorganic nanoparticles have a particle size of 0.850 μm to 5.251 μm.
7. A preparation method of a degradable temporary plugging agent is characterized in that the temporary plugging agent is prepared by melting, blending and molding a polyester material and inorganic nanoparticles according to the formula of the temporary plugging agent disclosed by any one of claims 1-5.
8. The method of claim 7, comprising the steps of:
s1: preparation of polyester Material
Selecting at least two of polylactic acid ester, polyglycolide and polybutylene succinate, and mixing uniformly in advance according to a formula;
s2: melting and blending the polyester material and the inorganic nano particles;
processing the polyester material by a double-roller mixing roll, open-milling for 0.5-2.5 h at the temperature of 180-240 ℃, uniformly spraying the nano particles between the double rollers, and cooling after milling;
s3: and (4) setting the rotating speed of a ball milling barrel to be 200-500 r/min by using a ball mill to ball mill and form the cooled temporary plugging agent.
9. The production method according to claim 8, wherein in S3, the temporary plugging agent is formed into particles of 286.3 μm to 525.7 μm by ball mill pulverization after cooling.
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