Epoxy resin plugging material and use method thereof
By using epoxy resin sealing materials, polymers are generated through polycondensation reaction, the problem of low sealing strength of existing cement sealing materials in medium and low permeability formations is solved, and the effects of high sealing rate, excellent mechanical properties and long-term validity are achieved.
Patent Information
- Application Number
- CN202411697457.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-26
- Publication Date
- 2025-02-25
AI Technical Summary
The existing cement sealing materials have low sealing strength, low success rate and short validity period in medium and low permeability formations, which limits their application scope.
Epoxy resin-based blocking materials are used to mix through independently aliquoted component A and component B. Component A includes epoxy resin and glycerol ether, and component B includes polyetheramine, N-aminoethylpiperazine and 2,4,6-tris(dimethylaminomethyl)phenol. The polymer is generated through polycondensation reaction to achieve blocking.
It achieves high sealing rate and excellent mechanical properties, has a long validity period, high temperature resistance, compressive strength, and a high success rate. It is suitable for various temperature environments.
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Figure BDA0005152443670000061
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of building materials, and particularly relates to an epoxy resin plugging material and a use method thereof. Background Art
[0002] The existing plugging materials are generally cement plugging materials, which use their impermeability after solidification to plug the water. They are usually used to seal the lower layer of water with cement plugs; squeeze into the water layer to block water. Because of its low price and ability to be used at various temperatures, it is still being studied and used.
[0003] However, due to the large size of cement particles, it is difficult to enter the medium and low permeability formations. Therefore, when the water is blocked by squeezing into the water layer, the blocking strength is not high, the success rate is low, and the effective period is short. For a long time, the application scope of this type of blocking material has been greatly limited. Summary of the invention
[0004] The object of the present invention is to provide an epoxy resin plugging material and a use method thereof. The epoxy resin plugging material provided by the present invention has a high plugging rate, excellent mechanical properties and a long effective period.
[0005] In order to achieve the above object, the present invention provides the following technical solutions:
[0006] The present invention provides an epoxy resin plugging material, comprising independently packaged component A and component B;
[0007] The component A comprises epoxy resin and glycerol ether;
[0008] The epoxy resin includes bisphenol A epoxy resin or bisphenol F epoxy resin;
[0009] When the epoxy resin is a bisphenol A epoxy resin, the glycerol ether includes 1,4-butanediol glycidyl ether and phenyl glycidyl ether; the component B includes polyetheramine, N-aminoethylpiperazine and 2,4,6-tris(dimethylaminomethyl)phenol;
[0010] When the epoxy resin is a bisphenol F type epoxy resin, the glycerol ether includes C12-14 alkyl glycidyl ether; and the component B includes a modified polyether amine curing agent or a modified alicyclic amine curing agent.
[0011] Preferably, when the epoxy resin is a bisphenol A epoxy resin, the component A comprises the following components in percentage by weight: 89.1 to 95.2% of bisphenol A epoxy resin, 2.0 to 5.0% of 1,4-butanediol glycidyl ether, and 2.0 to 6.0% of phenyl glycidyl ether;
[0012] The component B comprises the following components in percentage by mass: 80-92% of polyetheramine, 9-19% of N-aminoethylpiperazine and 0.1-0.8% of 2,4,6-tris(dimethylaminomethyl)phenol.
[0013] Preferably, when the epoxy resin is a bisphenol F epoxy resin, the component A comprises the following components in percentage by weight: 89.1 to 95.2% of bisphenol F epoxy resin and 4 to 11% of C12-14 alkyl glycidyl ether.
[0014] Preferably, when the epoxy resin is bisphenol A epoxy resin, the viscosity of component A after coating with a four-cup coating at 20° C. is 65 to 85 seconds; the viscosity of component B after coating with a four-cup coating at 20° C. is 11 to 20 seconds.
[0015] Preferably, when the epoxy resin is a bisphenol A epoxy resin, the preparation method of the component A comprises: performing a first mixing and stirring of the components to obtain the component A; the speed of the first mixing and stirring is 600 to 800 rpm, and the time is 30 to 40 minutes;
[0016] The preparation method of the component B comprises: performing a second stirring and mixing of the components to obtain the component B; the second mixing and stirring is performed at a rotation speed of 600 to 800 rpm for 30 to 40 minutes.
[0017] Preferably, when the epoxy resin is bisphenol F epoxy resin, the coating viscosity of component A at 20°C is 50 to 65s;
[0018] The viscosity of the component B in a coating cup at 20° C. is 30 to 40 seconds.
[0019] Preferably, when the epoxy resin is a bisphenol F epoxy resin, the preparation method of the component A comprises: subjecting the components to a third mixing process to obtain the component A; the rotation speed of the third mixing process is preferably 600 to 800 rpm, and the time is preferably 30 to 40 min.
[0020] Preferably, the mass ratio of component A to component B is 2 to 3:1.
[0021] The present invention also provides a method for using the epoxy resin plugging material described in the above technical solution, comprising the following steps:
[0022] The component A and the component B are mixed, and the obtained slurry is used for grouting the area to be blocked, and then solidified into gel.
[0023] Preferably, the slurry has a coating viscosity of 31 to 38 seconds at 25°C.
[0024] The temperature of the gelling and curing is 45-50° C., and the time is 90-120 minutes.
[0025] The invention provides an epoxy resin plugging material, comprising independently packaged component A and component B; the component A comprises epoxy resin and glycerol ether; the epoxy resin comprises bisphenol A epoxy resin or bisphenol F epoxy resin; when the epoxy resin is bisphenol A epoxy resin, the glycerol ether comprises 1,4-butanediol glycidyl ether and phenyl glycidyl ether; the component B comprises polyetheramine, N-aminoethylpiperazine and 2,4,6-tris(dimethylaminomethyl)phenol; when the epoxy resin is bisphenol F epoxy resin, the glycerol ether comprises C12-14 alkyl glycidyl ether; the component B comprises a modified polyetheramine curing agent or a modified alicyclic amine curing agent.
[0026] The present invention provides a novel solvent-free epoxy resin plugging material, which is a high molecular polymer produced by polycondensation reaction of low molecular substances, has a delayed gel reaction time and a long construction operation time; because it is immiscible with water, it can be used to drive water and fix sand in water-saturated sand bodies, and plug them by using its impermeability after solidification, and has low heat release during solidification, and will not cause physical structural damage to the object being used. Compared with existing cement plugging materials, it has the advantages of long-term temperature resistance (temperature at 45-85°C), high compressive strength (pressure at 30-50MPa), high plugging strength, high success rate and long validity period. DETAILED DESCRIPTION
[0027] The present invention provides an epoxy resin plugging material, comprising independently packaged component A and component B;
[0028] The component A comprises epoxy resin and glycerol ether;
[0029] The epoxy resin includes bisphenol A epoxy resin or bisphenol F epoxy resin;
[0030] When the epoxy resin is a bisphenol A epoxy resin, the glycerol ether includes 1,4-butanediol glycidyl ether and phenyl glycidyl ether; the component B includes polyetheramine, N-aminoethylpiperazine and 2,4,6-tris(dimethylaminomethyl)phenol;
[0031] When the epoxy resin is a bisphenol F type epoxy resin, the glycerol ether includes C12-14 alkyl glycidyl ether; and the component B includes a modified polyether amine curing agent or a modified alicyclic amine curing agent.
[0032] In the present invention, when the epoxy resin is a bisphenol A epoxy resin, the component A preferably includes the following components in percentage by mass: 89.1-95.2% of bisphenol A epoxy resin, 2.0-5.0% of 1,4-butanediol glycidyl ether and 2.0-6.0% of phenyl glycidyl ether, and further preferably includes 89.5-93% of bisphenol A epoxy resin, 3.0-4.5% of 1,4-butanediol glycidyl ether and 3.0-5.0% of phenyl glycidyl ether. In the present invention, the bisphenol A epoxy resin is preferably purchased from Shanghai Yuanbang Chemical, and the specific model is preferably 128 epoxy resin; the 1,4-butanediol glycidyl ether is preferably purchased from Jiangsu Sanmu Chemical; the phenyl glycidyl ether is preferably purchased from Jiangsu Sanmu Chemical. In the present invention, when the epoxy resin is a bisphenol A epoxy resin, the coating viscosity of the component A at 20°C is preferably 65-85s. In the present invention, the preparation method of the component A preferably comprises: performing a first stirring and mixing of the components to obtain the component A; the rotation speed of the first mixing and stirring is preferably 600 to 800 rpm, and the time is preferably 30 to 40 min.
[0033] In the present invention, when the epoxy resin is a bisphenol A epoxy resin, the component B preferably includes the following components in percentage by weight: 80-92% polyetheramine, 9-19% N-aminoethylpiperazine and 0.1-0.8% 2,4,6-tris(dimethylaminomethyl)phenol, and further preferably includes 85-90% polyetheramine, 12-14.5% N-aminoethylpiperazine and 0.3-0.5% 2,4,6-tris(dimethylaminomethyl)phenol. In the present invention, the polyetheramine is preferably purchased from Wanhua Chemical; the 2,4,6-tris(dimethylaminomethyl)phenol is preferably purchased from Jiangsu Sanmu Chemical.
[0034] In the present invention, when the epoxy resin is a bisphenol A epoxy resin, the coating viscosity of component B at 20°C is preferably 11 to 20 seconds. In the present invention, when the epoxy resin is a bisphenol A epoxy resin, the preparation method of component B preferably includes: subjecting the components to a second stirring and mixing to obtain component B; the second mixing and stirring is preferably performed at a speed of 600 to 800 rpm, and the time is preferably 30 to 40 minutes.
[0035] In the present invention, the specific model of the bisphenol F epoxy resin is preferably SMF170 epoxy resin. In the present invention, when the epoxy resin is bisphenol F epoxy resin, the component A preferably includes the following components in percentage by mass: 89.1-95.2% of bisphenol F epoxy resin, 4-11% of C12-14 alkyl glycidyl ether (AGE), and more preferably 89.5-93% of bisphenol F epoxy resin, 5-10.5% of C12-14 alkyl glycidyl ether. In the present invention, when the epoxy resin is bisphenol F epoxy resin, the 20°C coating viscosity of the component A is preferably 50-65s; the 20°C coating viscosity of the component B is preferably 30-40s.
[0036] In the present invention, the specific model of the modified polyetheramine curing agent is preferably 2293 curing agent; the specific model of the modified alicyclic amine curing agent is preferably 1085G-1 curing agent.
[0037] In the present invention, when the epoxy resin is a bisphenol F epoxy resin, the preparation method of the component A preferably includes: subjecting the components to a third mixing step to obtain the component A; the rotation speed of the third mixing step is preferably 600 to 800 rpm, and the time is preferably 30 to 40 min.
[0038] In the present invention, the mass ratio of component A to component B is preferably 2 to 3:1.
[0039] The present invention also provides a method for using the epoxy resin plugging material described in the above technical solution, comprising the following steps:
[0040] The component A and the component B are mixed, and the obtained slurry is used for grouting the area to be blocked, and then the slurry is cured into gel.
[0041] In the present invention, the coating viscosity of the slurry at 25° C. is preferably 31 to 38 seconds. In the present invention, the gelling and curing temperature is preferably 45 to 50° C., and the curing time is preferably 90 to 120 minutes.
[0042] Unless otherwise specified, the materials and equipment used in the present invention are all commercially available products in the art.
[0043] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0044] Example 1
[0045] Preparation:
[0046] Component A: 89.5% of bisphenol A epoxy resin (specific model is 128 epoxy resin), 4.5% of 1,4-butanediol glycidyl ether and 6.0% of phenyl glycidyl ether; add the above materials into a clean mixing tank in order, stir at 800rpm for 30 minutes, and measure the viscosity after stirring evenly. The viscosity is between 65 and 85 seconds (coating four cups at 20°C). After passing the test, package and obtain component A;
[0047] Component B: 85% polyetheramine, 14.5% N-aminoethylpiperazine and 0.5% 2,4,6-tris(dimethylaminomethyl)phenol; add the above materials into a clean mixing tank in order, stir at 800rpm for 30min, and measure the viscosity after stirring evenly. The viscosity is between 11 and 20 seconds (coating four cups at 20℃). If qualified, package and obtain component B;
[0048] The component A and the component B are mixed in a mass ratio of 3:1, and the obtained slurry is poured into the area to be plugged, followed by gelling and curing to obtain the epoxy resin plugging material.
[0049] Example 2
[0050] Component A: 89.5% of bisphenol F epoxy resin (specific model: SMF170 epoxy resin), 10.5% of C12-14 alkyl glycidyl ether (AGE); add the above materials into a clean mixing tank in order, stir at 800 rpm for 30 minutes, and measure the viscosity after stirring evenly. The viscosity is between 50 and 65 seconds (coating four cups at 20°C). After passing the test, package and obtain component A;
[0051] Component B: 100% modified alicyclic amine (specific model: 1085G-1 curing agent). Add the above materials into a clean mixing tank. The viscosity is between 30 and 35 seconds (coating four cups at 20°C). After passing the test, package and obtain component B.
[0052] The component A and the component B are mixed in a mass ratio of 3:1, and the obtained slurry is poured into the area to be plugged, followed by gelling and curing in sequence to obtain the epoxy resin plugging material.
[0053] Example 3
[0054] Component A: 89.5% of bisphenol F epoxy resin (specific model: SMF170 epoxy resin), 10.5% of C12-14 alkyl glycidyl ether (AGE); add the above materials into a clean mixing tank in order, stir at 800 rpm for 30 minutes, and measure the viscosity after stirring evenly. The viscosity is between 50 and 65 seconds (coating four cups at 20°C). After passing the test, package and obtain component A;
[0055] Component B: 100% modified polyetheramine (specific model: 2293 curing agent). Add the above materials into a clean mixing tank. The viscosity is between 35 and 40 seconds (coating four cups at 20°C). After passing the test, package and obtain component B.
[0056] The component A and the component B are mixed in a mass ratio of 2:1, and the obtained slurry is poured into the area to be plugged, followed by gelling and curing in sequence to obtain the epoxy resin plugging material.
[0057] Comparative Example 1
[0058] Preparation:
[0059] Component A: bisphenol A epoxy resin (specific model is 128 epoxy resin);
[0060] Component B: polyetheramine;
[0061] The component A and the component B are mixed in a mass ratio of 3:1, and the obtained slurry is poured into the area to be plugged, followed by gelling and curing in sequence to obtain the epoxy resin plugging material.
[0062] Comparative Example 2
[0063] Preparation:
[0064] Component A: 95% bisphenol A epoxy resin (specific model: 128 epoxy resin), 2.5% 1,4-butanediol glycidyl ether and 2.5% phenyl glycidyl ether; add the above materials into a clean mixing tank in order, stir at 800rpm for 30 minutes, and measure the viscosity after stirring evenly. The viscosity is between 65 and 85 seconds (coating four cups at 20°C). After passing the test, package and obtain component A;
[0065] Component B: polyetheramine;
[0066] The component A and the component B are mixed in a mass ratio of 3:1, and the obtained slurry is grouted in the area to be blocked, followed by gelling and curing in sequence to obtain the epoxy resin curing material.
[0067] Performance Testing
[0068] The performance of the plugging materials obtained in the examples and comparative examples was tested with reference to the following standards, wherein:
[0069] 1. Viscosity test standard: GB / T 1723-93;
[0070] 2. The initial gelling time refers to the test standard: 7.7 in JC / T 2037-2010;
[0071] 3. Compressive strength refers to the test standard: 7.9 in JC / T 2037-2010;
[0072] 4. Shore hardness test standard GB / T 2411-2008;
[0073] 5. The test method of plugging rate refers to SY / T 5336-2006;
[0074] 6. Construction performance is based on the coating viscosity of the plugging agent mixed material. If the viscosity is ≥100 seconds, it is difficult to construct; if the viscosity is between 60 and 100 seconds, it is relatively easy to construct; if the viscosity is less than 60 seconds, it is easy to construct;
[0075] The test results obtained are shown in Table 1;
[0076] Table 1 Performance test results of plugging materials obtained in Examples and Comparative Examples
[0077]
[0078]
[0079] It can be seen that the slurry obtained in the present application has moderate viscosity, a long initial gelling time, is easy to construct, has high long-term compressive strength (≥45MPa) after 24h curing, and has a plugging rate of up to 100%.
[0080] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments can be obtained based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.
Claims
1. An epoxy resin plugging material, characterized in that: Comprising independently packaged component A and component B; The component A comprises epoxy resin and glycerol ether; The epoxy resin includes bisphenol A epoxy resin or bisphenol F epoxy resin; When the epoxy resin is a bisphenol A epoxy resin, the glycerol ether includes 1,4-butanediol glycidyl ether and phenyl glycidyl ether; the component B includes polyetheramine, N-aminoethylpiperazine and 2,4,6-tris(dimethylaminomethyl)phenol; When the epoxy resin is a bisphenol F type epoxy resin, the glycerol ether includes C12-14 alkyl glycidyl ether; and the component B includes a modified polyether amine curing agent or a modified alicyclic amine curing agent.
2. The epoxy resin plugging material according to claim 1, characterized in that: When the epoxy resin is a bisphenol A epoxy resin, the component A comprises the following components in percentage by weight: 89.1 to 95.2% of bisphenol A epoxy resin, 2.0 to 5.0% of 1,4-butanediol glycidyl ether, and 2.0 to 6.0% of phenyl glycidyl ether; The component B comprises the following components in percentage by mass: 80-92% of polyetheramine, 9-19% of N-aminoethylpiperazine and 0.1-0.8% of 2,4,6-tris(dimethylaminomethyl)phenol.
3. The epoxy resin plugging material according to claim 1, characterized in that: When the epoxy resin is a bisphenol F epoxy resin, the component A comprises the following components in percentage by weight: 89.1 to 95.2% of bisphenol F epoxy resin and 4 to 11% of C12-14 alkyl glycidyl ether.
4. The epoxy resin plugging material according to claim 2, characterized in that: When the epoxy resin is bisphenol A epoxy resin, the viscosity of component A after coating with a four-cup coating at 20° C. is 65 to 85 seconds; the viscosity of component B after coating with a four-cup coating at 20° C. is 11 to 20 seconds.
5. The epoxy resin plugging material according to claim 1 or 4, characterized in that: When the epoxy resin is a bisphenol A epoxy resin, the preparation method of the component A comprises: performing a first mixing and stirring of the components to obtain the component A; the speed of the first mixing and stirring is 600 to 800 rpm, and the time is 30 to 40 minutes; The preparation method of the component B comprises: performing a second stirring and mixing of the components to obtain the component B; the second mixing and stirring is performed at a rotation speed of 600 to 800 rpm for 30 to 40 minutes.
6. The epoxy resin plugging material according to claim 3, characterized in that: When the epoxy resin is bisphenol F epoxy resin, the coating viscosity of component A at 20° C. is 50 to 65 seconds; The viscosity of the component B in a coating cup at 20° C. is 30 to 40 seconds.
7. The epoxy resin plugging material according to claim 1 or 6, characterized in that: When the epoxy resin is bisphenol F epoxy resin, the preparation method of component A comprises: performing a third mixing process on the components to obtain component A; the rotation speed of the third mixing process is preferably 600 to 800 rpm, and the time is preferably 30 to 40 minutes.
8. The epoxy resin plugging material according to claim 1, characterized in that: The mass ratio of component A to component B is 2-3:
1.
9. The method for using the epoxy resin plugging material according to any one of claims 1 to 8, characterized in that: The following steps are involved: The component A and the component B are mixed, and the obtained slurry is used for grouting the area to be blocked, and then solidified into gel.
10. The method of use according to claim 9, characterized in that: The viscosity of the slurry at 25°C is 31-38s; The temperature of the gelling and curing is 45-50° C., and the time is 90-120 minutes.
Citation Information
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