CN111484579B - High-temperature soluble bridge plug and preparation method thereof - Google Patents
High-temperature soluble bridge plug and preparation method thereof Download PDFInfo
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- CN111484579B CN111484579B CN202010301152.0A CN202010301152A CN111484579B CN 111484579 B CN111484579 B CN 111484579B CN 202010301152 A CN202010301152 A CN 202010301152A CN 111484579 B CN111484579 B CN 111484579B
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- temperature soluble
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- 238000002360 preparation method Methods 0.000 title abstract description 8
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002994 raw material Substances 0.000 claims abstract description 25
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000003349 gelling agent Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000009757 thermoplastic moulding Methods 0.000 claims abstract description 3
- FZERHIULMFGESH-UHFFFAOYSA-N N-phenylacetamide Chemical group CC(=O)NC1=CC=CC=C1 FZERHIULMFGESH-UHFFFAOYSA-N 0.000 claims description 24
- 229960001413 acetanilide Drugs 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- KZQUJFQCBZWDGP-UHFFFAOYSA-N 2,2-dinitrobutanenitrile Chemical group [N+](=O)([O-])C(C#N)(CC)[N+](=O)[O-] KZQUJFQCBZWDGP-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007789 gas Substances 0.000 abstract description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005553 drilling Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 5
- 229920001577 copolymer Polymers 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- TUECBOWWQQEEDA-UHFFFAOYSA-N C(CCC)#N.[N].[N] Chemical compound C(CCC)#N.[N].[N] TUECBOWWQQEEDA-UHFFFAOYSA-N 0.000 abstract description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract 4
- 230000009471 action Effects 0.000 description 22
- 239000000243 solution Substances 0.000 description 22
- 238000004090 dissolution Methods 0.000 description 15
- 229920000642 polymer Polymers 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000012265 solid product Substances 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 5
- UWDOAGAVGKNYJR-UHFFFAOYSA-N [N+](=[N-])=C(C#N)CC Chemical compound [N+](=[N-])=C(C#N)CC UWDOAGAVGKNYJR-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 231100000331 toxic Toxicity 0.000 description 4
- 230000002588 toxic effect Effects 0.000 description 4
- NLPNDKUSBJCVAE-UHFFFAOYSA-N (diazonioamino)ethane Chemical compound CCN[N+]#N NLPNDKUSBJCVAE-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000007281 self degradation Effects 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/04—Anhydrides, e.g. cyclic anhydrides
- C08F222/06—Maleic anhydride
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
- E21B33/134—Bridging plugs
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- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Geochemistry & Mineralogy (AREA)
- Fluid Mechanics (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high-temperature soluble bridge plug and a preparation method thereof, and the preparation method comprises the following steps: 1) taking butadiene and maleic anhydride, adding an anti-gelling agent, adding dinitrogen-butyronitrile, dissolving in DMF (dimethyl formamide) as an initiator, adding KH570 as a coupling agent and DMF as a solvent; heating in a constant-temperature oil bath under the protection of nitrogen, and fully performing reflux reaction at 140-180 ℃; 2) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is the raw material for the high-temperature soluble bridge plug; and carrying out thermoplastic molding on the obtained raw materials by using a mold to prepare the high-temperature soluble bridge plug. The invention fully utilizes the characteristics of high temperature resistance, pressure resistance and water solubility of the copolymer synthesized by maleic anhydride and butadiene, finally degrades the copolymer into water and carbon dioxide, reduces the reverse drainage process, and is a biodegradable environment-friendly material. The high-temperature soluble bridge plug can be applied to the development of unconventional gas reservoirs such as external shale gas, liquid in the well enables the high-temperature soluble bridge plug to be dissolved automatically, shaft drilling and grinding operation and reverse arrangement treatment are not needed, and full-bore production of a shaft is achieved.
Description
Technical Field
The invention relates to a high-temperature soluble bridge plug, in particular to a high-temperature soluble bridge plug and a preparation method thereof.
Background
Generally, the soluble bridge plug is dissolved automatically in a liquid environment in a well under a certain temperature condition after construction is finished, and the full-drift-diameter production of the well is realized without well drilling and grinding operation. Maleic anhydride is used as a common basic organic chemical monomer raw material, and carboxyl groups existing in a molecular structure of the maleic anhydride have good compatibility with polar solution, so that the maleic anhydride has great advantages in a dissolving process. The orthorhombic needle-shaped structure of the butadiene can enhance high-temperature resistance, wear resistance and smaller compression deformation. Therefore, the copolymer synthesized by maleic anhydride and butadiene is a polymer with polar groups in a molecular structure, has small specific gravity, strength similar to that of carbon steel, high temperature resistance and strong pressure resistance, can react with surrounding media and gradually dissolve, and can be used as a biodegradable environment-friendly material.
Disclosure of Invention
The invention aims to provide a high-temperature soluble bridge plug and a preparation method thereof. The stable interlayer packing is provided during fracturing, the bridge plug is not required to be drilled and ground after fracturing is completed, the self-degradation can be realized only by depending on the temperature change of liquid in a shaft, and the body disappears completely after dissolution. The higher the temperature in the degradation process, the faster the main chain of the high polymer is decomposed into oligomers, and unstable C-C bonds on the main chain of the high polymer are decomposed into the oligomers and finally degraded into carbon dioxide and water, so that toxic and harmful gases are not generated, and the inverted discharge cost is reduced. The method is particularly suitable for deep long horizontal section shale gas well operation. The strength and solubility of well condition conditions for targeted design are met. The high-temperature soluble bridge plug utilizes the characteristics of high temperature resistance, pressure resistance and water solubility of a copolymer synthesized by maleic anhydride and butadiene, is finally degraded into water and carbon dioxide, reduces the reverse drainage process, and is a biodegradable environment-friendly material.
The technical scheme adopted by the invention is as follows:
the high-temperature soluble bridge plug under the action of high temperature is characterized by having the following structure:
the value range of n is 1000-10000.
The high-temperature soluble bridge plug under the high-temperature action is high-temperature resistant and high in pressure resistance, can react with surrounding media and gradually dissolve, can be automatically degraded only by means of temperature change in a shaft, completely disappears after dissolution, and the higher the temperature of a salt solution in the degradation process is, the faster the main chain of a high polymer is decomposed into an oligomer, and toxic and harmful gas cannot be generated.
The high-temperature soluble bridge plug under the high-temperature action is synthesized by polymerization reaction of maleic anhydride and butadiene, the diazobutyronitrile is used as an initiator, the acetanilide is used as an antigelling agent, and the KH570 is used as a coupling agent, so that the bonding strength of the coupling agent and the acetanilide can be improved. The synthesis mechanism is as follows:
the value range of n is 1000-10000.
The high-temperature soluble bridge plug is made of a high-temperature soluble material; the high temperature is 80-180 ℃.
A preparation method of a high-temperature soluble bridge plug comprises the following steps:
1) taking butadiene and maleic anhydride, and adding an antigelling agent, an initiator, a coupling agent and a solvent; heating in a constant-temperature oil bath under the protection of nitrogen, and fully performing reflux reaction at 140-180 ℃;
2) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is the raw material for the high-temperature soluble bridge plug; and carrying out thermoplastic molding on the obtained raw materials by using a mold to prepare the high-temperature soluble bridge plug.
3) And weighing KCl, and preparing a 3-5% solution as the environment of the bridge plug.
4) The prepared high-temperature soluble bridge plug raw material under the high-temperature action is put into a 3-5% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
The raw material of the high-temperature soluble bridge plug under the high-temperature action prepared by the method can be used as the high-temperature soluble bridge plug to be applied to the development of unconventional gas reservoirs such as external shale gas and the like.
Preferably, the initiator is the diazoniabutyronitrile, and the addition amount accounts for 2-4% of the total amount of the monomers.
Preferably, the coupling agent is KH570, and the addition amount accounts for 1-1.5% of the total amount of the monomers.
Preferably, the mass of the maleic anhydride is 2-3 times that of butadiene.
Preferably, the anti-gelling agent is acetanilide, and the addition amount of the anti-gelling agent accounts for 4-5% of the total amount of the monomers.
Preferably, the solvent is DMF.
Compared with the prior art, the invention has the following advantages:
the invention provides a high-temperature soluble bridge plug under the action of high temperature. The high-temperature soluble bridge plug is small in specific gravity, the strength is close to that of carbon steel, the dissolving rate is mainly influenced by the liquid temperature, the dissolving time is controllable and adjustable, the body disappears completely after dissolving, no residue is generated on the sleeve, the higher the temperature of the salt solution is in the degradation process, the faster the high polymer main chain is decomposed into low polymers, and no toxic and harmful gas is generated. After fracturing is completed, liquid drainage and yield seeking can be completed without drilling and grinding a bridge plug, and working hours and operation cost are saved. The method is particularly suitable for deep long horizontal section shale gas well operation.
The invention is synthesized by polymerization reaction of butadiene and maleic anhydride by using coupling dinitrogen butyronitrile as an initiator, acetanilide as an antigelling agent and KH570 as a coupling agent; the maleic anhydride has a great advantage in the dissolution process because of the good compatibility with polar solutions due to the carboxyl groups present in the molecular structure of maleic anhydride. The orthorhombic needle-shaped structure of the butadiene can enhance high-temperature resistance, wear resistance and smaller compression deformation. Therefore, the copolymer synthesized by maleic anhydride and butadiene has the characteristics of high temperature resistance, pressure resistance and water solubility, and is finally degraded into water and carbon dioxide, so that the reverse drainage process is reduced, the operation aging is obviously improved, and the drilling and plugging operation risk and cost are reduced. Therefore, the high-temperature soluble bridge plug can be applied to the development of unconventional gas reservoirs such as external shale gas, liquid in a well enables the high-temperature soluble bridge plug to be dissolved automatically, well bore drilling and grinding operation is not needed, and full-bore production of a well bore is achieved.
The high molecular polymer can replace a high-temperature soluble bridge plug made of a magnesium-aluminum alloy material, and under the condition that the advantages of the high-temperature soluble bridge plug made of the magnesium-aluminum alloy material are kept, the dissolution rate of the high molecular polymer is only influenced and controllable by temperature, and the higher the temperature is, the faster the dissolution is. Finally, the water and the carbon dioxide are degraded, the reverse drainage process is reduced, the operation timeliness is obviously improved, and the drilling and plugging operation risk and cost are reduced.
Detailed Description
The invention relates to a high-temperature soluble bridge plug under the action of high temperature, which comprises the following specific preparation processes:
the reaction equation of the synthesis of the high-temperature soluble bridge plug under the action of high temperature is as follows:
the value range of n is 1000-10000.
According to the above reaction mechanism, the method comprises the steps of:
(1) weighing a certain amount of butadiene and maleic anhydride, adding acetanilide accounting for 4-5% of the total amount of the monomers to serve as an anti-gelling agent, dissolving azodicarbonitrile in DMF accounting for 2-4% of the total amount of the monomers to serve as an initiator, taking KH570 accounting for 1-1.5% of the total amount of the monomers to serve as a coupling agent, taking DMF as a solvent, and taking the mass of the maleic anhydride to be 2-3 times that of butadiene. Pouring the mixture into a 500mL three-necked bottle with a stirrer, heating the mixture in a nitrogen-protected constant-temperature oil bath, refluxing the mixture for 4 to 6 hours at the temperature of between 140 and 180 ℃, and cooling the mixture.
(2) And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
(3) And weighing KCl, and preparing a 3-5% solution as the environment of the bridge plug.
(4) The prepared high-temperature soluble bridge plug raw material under the high-temperature action is put into a 3-5% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
The present invention will be described in detail with reference to the following specific examples:
example 1
3g of butadiene and 6g of maleic anhydride, 0.09g of KH570 as a coupling agent, 0.36g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, the solution is poured into a 500mL three-necked bottle with a stirrer and is protected by nitrogen, and the temperature is raised to 140 ℃. 0.18g of the diazobutyronitrile is dissolved in 5g of DMF and poured into a constant-pressure separating funnel to be dripped out for two hours to be used as an initiator. Then refluxed at 140 ℃ for 4h, the reaction was stopped and cooled.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
6g of KCl is weighed and dissolved in 200g of water to prepare a 3% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into 3 percent KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Example 2
3g of butadiene and 9g of maleic anhydride and 0.12g of KH570 as coupling agents and 0.48g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, and the mixture is poured into a 500mL three-necked bottle with a stirrer and is heated to 180 ℃ under the protection of nitrogen. 0.24g of the diazoniabutyronitrile is dissolved in 5g of DMF and poured into a constant-pressure separating funnel to be dripped out for two hours to be used as an initiator. Then refluxing at 180 deg.C for 6h, stopping reaction, and cooling.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
8g of KCl is weighed and dissolved in 200g of water to prepare a 4% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into a 4% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Example 3
3g of butadiene and 9g of maleic anhydride, 0.18g of KH570 as a coupling agent and 0.48g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, and the mixture is poured into a 500mL three-necked bottle with a stirrer and is heated to 180 ℃ under the protection of nitrogen. 0.48g of the diazonitrile was dissolved in 5g of DMF and poured into a constant pressure separatory funnel and dripped off for two hours to serve as an initiator. Then refluxed at 180 ℃ for 4 hours, the reaction was stopped, and cooled.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
10g of KCl is weighed and dissolved in 200g of water to prepare a 5% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into a 5% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Example 4
3g of butadiene and 6g of maleic anhydride, 0.135g of KH570 as a coupling agent, 0.45g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, the solution is poured into a 500mL three-necked bottle with a stirrer and is protected by nitrogen, and the temperature is raised to 140 ℃. 0.27g of the diazobutyronitrile is dissolved in 5g of DMF and poured into a constant-pressure separating funnel to be dripped out for two hours to be used as an initiator. Then refluxed at 140 ℃ for 6h, the reaction was stopped and cooled.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
8g of KCl is weighed and dissolved in 200g of water to prepare a 4% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into a 4% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Example 5
3g of butadiene and 9g of maleic anhydride, 0.12g of KH570 as a coupling agent and 0.6g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, and the mixture is poured into a 500mL three-necked bottle with a stirrer and is heated to 160 ℃ under the protection of nitrogen. 0.24g of the diazoniabutyronitrile is dissolved in 5g of DMF and poured into a constant-pressure separating funnel to be dripped out for two hours to be used as an initiator. Then refluxed at 160 ℃ for 4 hours, the reaction was stopped, and cooled.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
10g of KCl is weighed and dissolved in 200g of water to prepare a 5% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into a 5% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Example 6
3g of butadiene and 6g of maleic anhydride, 0.09g of KH570 as a coupling agent, 0.45g of acetanilide as an antigelling agent are respectively weighed and dissolved in 15g of DMF, the solution is poured into a 500mL three-necked bottle with a stirrer and is protected by nitrogen, and the temperature is raised to 150 ℃. 0.27g of the diazobutyronitrile is dissolved in 5g of DMF and poured into a constant-pressure separating funnel to be dripped out for two hours to be used as an initiator. Then refluxed at 150 ℃ for 6 hours, the reaction was stopped, and cooled.
And (3) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is a product used for the high-temperature soluble bridge plug under the action of high temperature. The obtained solid product was molded into a cylindrical shape having a bottom area radius of 1cm and a height of 5 cm. And (6) carrying out testing.
10g of KCl is weighed and dissolved in 200g of water to prepare a 5% solution which is used as the environment where the bridge plug works.
The prepared high-temperature soluble bridge plug raw material under the action of high temperature is put into a 5% KCl solution, and the dissolution time of the raw material at six different temperatures of 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ is tested and recorded.
Table 1 shows the results of the high temperature soluble bridge plug test of example 4.
| Temperature (. degree.C.) | Degradation time (d) |
| At room temperature | 15 |
| 80 | 9 |
| 100 | 8 |
| 120 | 6 |
| 140 | 5 |
| 160 | 4 |
| 180 | 2 |
Table 1 shows the results of performance tests performed on one of the high temperature soluble bridge plugs and the method of making the same in example 4. As can be seen from the table, when this high temperature soluble bridge plug was dissolved at room temperature, the high temperature soluble bridge plug was completely dissolved for 15 days, indicating that the bridge plug was soluble. When the temperature of the high-temperature soluble bridge plug rises in the KCl solution, the dissolution time of the high-temperature soluble bridge plug is shorter, because the carboxylic acid dissolution speed of the high-temperature soluble bridge plug polymer is increased. The higher the temperature in the degradation process, the faster the main chain of the high polymer is decomposed into oligomers, no toxic and harmful gas is generated, and the inverted discharge cost is reduced.
The foregoing is a more detailed description of the invention and it is not intended that the invention be limited to the specific embodiments described herein, but that various modifications, alterations, and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be construed to fall within the scope of the invention as defined by the appended claims.
Claims (6)
1. A high temperature soluble bridge plug characterized by: the material of the high-temperature soluble bridge plug has the following structural formula:
the value range of n is 1000-10000;
the mass of maleic anhydride in the monomer used by the high-temperature soluble bridge plug raw material is 2-3 times that of butadiene.
2. A method of making a high temperature soluble bridge plug according to claim 1, comprising the steps of:
1) taking butadiene and maleic anhydride as monomers, and adding an antigelling agent, an initiator, a coupling agent and a solvent; heating in a constant-temperature oil bath under the protection of nitrogen, and fully performing reflux reaction at 140-180 ℃;
2) centrifugally washing the solid-liquid mixture after the reaction, and drying in vacuum to obtain light yellow solid which is the raw material for the high-temperature soluble bridge plug; and carrying out thermoplastic molding on the obtained raw materials by using a mold to prepare the high-temperature soluble bridge plug.
3. The method for preparing the high-temperature soluble bridge plug as claimed in claim 2, wherein the initiator is dinitrobutyronitrile, and the addition amount of the initiator accounts for 2-4% of the total mass of the monomers.
4. The method for preparing the high-temperature soluble bridge plug as claimed in claim 2, wherein the coupling agent is KH570, and the addition amount of the coupling agent accounts for 1-1.5% of the total mass of the monomers.
5. The method for preparing the high-temperature soluble bridge plug as claimed in claim 2, wherein the anti-gelling agent is acetanilide, and the addition amount of the anti-gelling agent accounts for 4-5% of the total mass of the monomers.
6. The method of claim 2, wherein the solvent is DMF.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| GB1219256A (en) * | 1968-04-26 | 1971-01-13 | Borg Warner | Method of copolymerizing unhindered conjugated dienes with maleic anhydride |
| CN101781387B (en) * | 2010-03-22 | 2012-06-20 | 北京化工大学 | Method for copolymerization of maleic anhydride/conjugated diene |
| CN103304736B (en) * | 2013-06-13 | 2015-09-23 | 中国海洋石油总公司 | A kind of preparation method of water soluble dispersing agent |
| US20170306144A1 (en) * | 2014-11-13 | 2017-10-26 | Kureha Corporation | Polyglycolic acid resin composition, molded product for well drilling, and downhole tool member |
| CN109160974B (en) * | 2018-07-27 | 2020-12-15 | 天津安浩生物科技有限公司 | Aqueous phase preparation method of maleic anhydride-conjugated diene copolymer |
| CN109826592A (en) * | 2019-02-16 | 2019-05-31 | 陕西海格瑞恩实业有限公司 | A kind of short and small complete solvable bridge plug suitable for varying environment |
| CN110513076A (en) * | 2019-09-24 | 2019-11-29 | 中国石油集团西部钻探工程有限公司 | The solvable bridge plug of pressure break metal sealing |
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