CN115595133A - Composition for dissolving plugging agent and preparation method and application thereof - Google Patents
Composition for dissolving plugging agent and preparation method and application thereof Download PDFInfo
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- CN115595133A CN115595133A CN202110766853.6A CN202110766853A CN115595133A CN 115595133 A CN115595133 A CN 115595133A CN 202110766853 A CN202110766853 A CN 202110766853A CN 115595133 A CN115595133 A CN 115595133A
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- mixed solution
- composition
- dissolving
- plugging agent
- corrosion inhibitor
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
Abstract
The invention discloses a composition for dissolving a plugging agent, and a preparation method and application thereof. The composition comprises dichloromethane, phenol, hydrochloric acid, ammonia nitrogen water and a corrosion inhibitor. The composition comprises, by taking the total mass of the composition as 100%, 75-85% of dichloromethane, 3-6% of phenol, 5-15% of hydrochloric acid, 2-6% of ammonia nitrogen water and 1-2% of corrosion inhibitor.
Description
Technical Field
The invention provides a composition for dissolving an epoxy resin plugging agent, and a preparation method and application thereof.
Background
In oil and gas exploration and development, loss caused by well leakage reaches hundreds of millions of dollars every year around the world, and inestimable loss is brought to oil and gas well development. And the vicious leakage caused by loss-return leakage, karst cave leakage, broken stratum and the like can cause buried drilling, well collapse and even well abandonment, thereby seriously restricting the exploration and development process of the oil-gas well.
The epoxy resin plugging agent has the characteristics of normal-temperature pumpability, solidification time temperature control, high solidification compressive strength, obvious large crack plugging effect and the like, and has obvious advantages in the aspect of malignant leakage control technology. Meanwhile, the epoxy resin plugging agent belongs to a high molecular polymer with a three-dimensional space structure, is difficult to dissolve and remove, and is easy to generate safety accidents in oil and gas well production.
Aiming at the problem that no special dissolving agent exists in the epoxy resin plugging agent for the oil and gas well at present, the epoxy resin plugging agent cannot meet the requirements of quick dissolution and plugging removal after plugging operation of the oil and gas well.
Disclosure of Invention
The invention provides a composition for dissolving a plugging agent, which comprises dichloromethane, phenol, hydrochloric acid, ammonia nitrogen water and a corrosion inhibitor.
In a specific embodiment, based on 100% of the total mass of the composition, the content of the dichloromethane is 75% to 85%, the content of the phenol is 3% to 6%, the content of the hydrochloric acid is 5% to 15%, the content of the ammoniacal nitrogen water is 2% to 6%, and the content of the corrosion inhibitor is 1% to 2%.
In one embodiment, the corrosion inhibitor is an imidazoline based pickling corrosion inhibitor.
In one embodiment, the corrosion inhibitor is a modified alkyl imidazoline quaternary ammonium salt type corrosion inhibitor MZL-A.
In a specific embodiment, the hydrochloric acid has a hydrogen chloride content of 36 to 38% by mass.
In a specific embodiment, the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The second aspect of the invention provides a process for the preparation of a composition according to any one of the first to the second aspects of the invention, comprising:
1) Uniformly mixing the hydrochloric acid and the ammonia nitrogen water according to the mass ratio of 2.5;
2) Adding the corrosion inhibitor into the first mixed solution, and uniformly mixing to obtain a second mixed solution;
3) Adding phenol into the second mixed solution, and uniformly mixing to obtain a third mixed solution;
4) And adding dichloromethane into the third mixed solution, and uniformly mixing to obtain the composition.
The third invention provides the use of the composition according to any one of the first invention or the composition prepared by the preparation method of the second invention in dissolving a plugging agent.
In one embodiment, the lost circulation agent is an epoxy lost circulation agent.
The invention has the beneficial effects that:
the composition for dissolving the plugging agent can quickly and effectively destroy the three-dimensional space structure of the epoxy resin plugging agent through the synergistic effect of the dichloromethane, the hydrochloric acid and the nitric acid, and achieves the purposes of swelling, dissolving and plugging removal. The dissolution rate of the epoxy resin plugging agent for 24 hours at 25 ℃ is 35.62 percent; along with the rise of the temperature, the dissolution rate of the epoxy resin plugging agent is gradually increased; when the temperature is increased from 25 ℃ to 150 ℃, the dissolution rate at 24h can be increased to 88.14 percent for example; as the dissolution time increases, the dissolution rate increases and gradually becomes stable. Meanwhile, the corrosion rate of the composition to the steel sheet (N80) is less than 0.01g/m at 150 ℃ due to the addition of the corrosion inhibitor 2 H. Compared with the existing epoxy resin dissolving agent, the developed composition has the advantages of high dissolving rate, small corrosivity to oil casings and the like for the epoxy resin plugging agent for oil and gas wells, meets the requirements of quick dissolving and plugging removal after plugging operation of the oil and gas wells, and effectively protects the safety production of the oil and gas wells.
In the present invention, the term "ammoniacal nitrogen water" refers to an aqueous solution of nitric acid.
Detailed Description
The present invention is further described below with reference to examples, which are intended to be illustrative only, and are not intended to limit the scope of the present invention in any way.
Unless otherwise specified, the above chemicals are all commercially available.
Example 1
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 15g of hydrochloric acid and 6g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 1g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: adding 3g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 75g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 2
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 12.5g of hydrochloric acid and 5g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 1g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 5.5g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 76g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 3
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 12.5g of hydrochloric acid and 5g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 1g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: adding 3.5g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 78g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 4
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 12.5g of hydrochloric acid and 5g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
step 2: adding 1g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 3g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 78.5g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 5
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 10g of hydrochloric acid and 4g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
step 2: adding 2g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 4g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 80g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 6
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 10g of hydrochloric acid and 4g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
step 2: adding 2g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 3g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: adding 81g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 7
The mass percentage of hydrogen chloride in the hydrochloric acid used in the embodiment is 36% to 38%; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 10g of hydrochloric acid and 4g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 1.5g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: adding 3g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: adding 81.5g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 8
The mass percentage of hydrogen chloride in the hydrochloric acid used in the embodiment is 36% to 38%; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 7.5g of hydrochloric acid and 3g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
step 2: adding 1.5g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: adding 6g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 82g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 9
The mass percentage of hydrogen chloride in the hydrochloric acid used in the embodiment is 36% to 38%; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 7.5g of hydrochloric acid and 3g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 1g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 3.5g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 85g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 10
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 5g of hydrochloric acid and 2g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 2g of corrosion inhibitor MZL-A into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: adding 6g of phenol into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 85g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Example 11
The mass percentage of the hydrogen chloride in the hydrochloric acid used in the embodiment is 36 to 38 percent; the mass percentage of the nitric acid in the ammonia nitrogen water is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 7.5g of hydrochloric acid and 3g of ammonia nitrogen water, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 4.5g of phenol into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: and adding 85g of dichloromethane into the second mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Comparative example 1
The compound used for dissolving the epoxy resin plugging agent is 100g of dichloromethane.
Comparative example 2
The hydrochloric acid used in this comparative example had a hydrogen chloride content of 36 to 38% by mass.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: uniformly stirring 10.5g of hydrochloric acid and 1g of corrosion inhibitor MZL-A to obtain a first mixed solution;
and 2, step: adding 3.5g of phenol into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: and adding 85g of dichloromethane into the second mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Comparative example 3
The mass percentage of the nitric acid in the ammonia nitrogen water used in the comparative example is 65-68%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: uniformly stirring 10.5g of ammonia nitrogen water and 1g of corrosion inhibitor MZL-A to obtain a first mixed solution;
and 2, step: adding 3.5g of phenol into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and 3, step 3: and adding 85g of dichloromethane into the second mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Comparative example 4
The mass percentage of sulfuric acid in the concentrated sulfuric acid used in this comparative example was 98.3%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 10.5g of concentrated sulfuric acid and 4.5g of phenol, and uniformly stirring to obtain a first mixed solution;
and 2, step: and adding 85g of dichloromethane into the first mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Comparative example 5
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 1.5g of sodium hydroxide and 20g of ethylene glycol monomethyl ether, and uniformly stirring to obtain a first mixed solution;
step 2: adding 10g of diethylenetriamine into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: adding 5g of toluene into the second mixed solution, and uniformly stirring to obtain a third mixed solution;
and 4, step 4: and adding 63.5g of dichloromethane into the third mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
Comparative example 6
The mass percentage of sulfuric acid in the concentrated sulfuric acid used in the comparative example was 98.3%.
The preparation method of the composition for dissolving the epoxy resin plugging agent comprises the following steps:
step 1: mixing 10g of formic acid and 4g of phenol, and uniformly stirring to obtain a first mixed solution;
and 2, step: adding 83.5g of dichloromethane into the first mixed solution, and uniformly stirring to obtain a second mixed solution;
and step 3: and adding 2.5g of sulfuric acid into the second mixed solution, and fully and uniformly stirring to obtain the composition for dissolving the epoxy resin plugging agent.
The compositions or compounds of the above examples and comparative examples were evaluated for dissolution rate and corrosion rate, and the specific experimental conditions and requirements were: 1) The dissolution rate experiment measures the dissolution condition of the composition to the epoxy resin plugging agent under the conditions of 150 ℃ and 24 hours; 2) The corrosion rate was measured at 150 ℃ for 24h and the results are shown in Table 1.
TABLE 1 evaluation of dissolution rate and Corrosion Rate
Note: "-" indicates no measurement.
As can be seen from Table 1, the compositions prepared by the above examples of the invention have a dissolution rate of more than 82.00% for the epoxy resin plugging agent at 150 ℃ for 24 h; the corrosion rate of the steel sheet (N80) at 150 ℃ is less than 0.01g/m 2 H. The dissolution rate of the epoxy resin plugging agent of the compositions prepared in comparative examples 1 to 3 is only 52.94% at most, and thus it can be seen that the dichloromethane in the composition of the present inventionThe alkane, the hydrochloric acid and the nitric acid generate a synergistic interaction effect, so that the dissolution of the epoxy resin plugging agent is accelerated. As can be seen from the comparison between examples 1 to 11 and comparative examples 4 and 6, the dissolution rate of the epoxy resin plugging agent is also significantly improved compared to the composition containing concentrated sulfuric acid due to the synergistic effect between the components of the composition of the present invention. In conclusion, the technical effect produced by the composition of the present invention is superior as a result of the synergistic effect between the components in the composition of the present invention, as analyzed by comparing examples with comparative examples.
While the invention has been described with reference to specific embodiments, those skilled in the art will appreciate that various changes can be made without departing from the true spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation, material, composition of matter, and method to the essential scope and spirit of the present invention. All such modifications are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (8)
1. A composition for dissolving a plugging agent comprises dichloromethane, phenol, hydrochloric acid, ammonia nitrogen water and a corrosion inhibitor.
2. The composition of claim 1, wherein the dichloromethane content is 75% to 85%, the phenol content is 3% to 6%, the hydrochloric acid content is 5% to 15%, the ammoniacal nitrogen water content is 2% to 6%, and the corrosion inhibitor content is 1% to 2%, based on 100% of the total mass of the composition.
3. The composition of claim 1, wherein the corrosion inhibitor is an imidazoline based pickling corrosion inhibitor; preferably, the corrosion inhibitor is a modified alkyl imidazoline quaternary ammonium salt corrosion inhibitor MZL-A.
4. The composition according to any one of claims 1 to 3, wherein the hydrochloric acid has a hydrogen chloride content of 36 to 38% by mass.
5. The composition according to any one of claims 1 to 4, wherein the mass percentage of the nitric acid in the ammonia nitrogen water is 65 to 68 percent.
6. A process for preparing a composition according to any one of claims 1 to 5, which comprises:
1) Uniformly mixing the hydrochloric acid and the ammonia nitrogen water according to the mass ratio of 2.5;
2) Adding the corrosion inhibitor into the first mixed solution, and uniformly mixing to obtain a second mixed solution;
3) Adding phenol into the second mixed solution, and uniformly mixing to obtain a third mixed solution;
4) And adding dichloromethane into the third mixed solution, and uniformly mixing to obtain the composition.
7. Use of a composition according to any one of claims 1 to 5 or prepared by the method of claim 6 in dissolving a plugging agent.
8. The use of claim 7, wherein the lost circulation agent is an epoxy lost circulation agent.
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| US4171240A (en) * | 1978-04-26 | 1979-10-16 | Western Electric Company, Inc. | Method of removing a cured epoxy from a metal surface |
| RU2182655C1 (en) * | 2001-08-23 | 2002-05-20 | Закрытое акционерное общество "РЕНФОРС" | Process of treatment of face zone of pool |
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| CN101649068A (en) * | 2008-08-12 | 2010-02-17 | 贵州航天林泉电机有限公司 | Epoxy resin dissolving agent and preparing method thereof |
| CN107099052A (en) * | 2017-04-25 | 2017-08-29 | 桂林电子科技大学 | A kind of cured epoxy resin lytic agent and its application process |
| CN112048292A (en) * | 2020-08-17 | 2020-12-08 | 中海油田服务股份有限公司 | Blockage removing liquid and application thereof |
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2021
- 2021-07-07 CN CN202110766853.6A patent/CN115595133A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4171240A (en) * | 1978-04-26 | 1979-10-16 | Western Electric Company, Inc. | Method of removing a cured epoxy from a metal surface |
| RU2182655C1 (en) * | 2001-08-23 | 2002-05-20 | Закрытое акционерное общество "РЕНФОРС" | Process of treatment of face zone of pool |
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| CN101649068A (en) * | 2008-08-12 | 2010-02-17 | 贵州航天林泉电机有限公司 | Epoxy resin dissolving agent and preparing method thereof |
| CN107099052A (en) * | 2017-04-25 | 2017-08-29 | 桂林电子科技大学 | A kind of cured epoxy resin lytic agent and its application process |
| CN112048292A (en) * | 2020-08-17 | 2020-12-08 | 中海油田服务股份有限公司 | Blockage removing liquid and application thereof |
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