CN103013052B - Degradable underground blocking material - Google Patents
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- CN103013052B CN103013052B CN201210548442.0A CN201210548442A CN103013052B CN 103013052 B CN103013052 B CN 103013052B CN 201210548442 A CN201210548442 A CN 201210548442A CN 103013052 B CN103013052 B CN 103013052B
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Abstract
The invention discloses a degradable underground blocking material, which belongs to the technical field of material preparation. The degradable underground blocking material is formed by components A and B, wherein the component A comprises epoxy resin, flexibilizer, a diluting agent, a coupling agent, a filler and a soluble or a degradable substance A; the component B comprises a hardener, a compound accelerant and a soluble or degradable substance B; and both soluble or the degradable substances A and B can be zero, but the soluble or the degradable substances A and B cannot be zero synchronously. The components A and B are mixed according to a weight ratio of 1:(0.15-0.35) when the material is in use. The invention has the benefits that after certain operation time, the material partially and automatically degrades or dissolves, environmental protection is facilitated; nonselective adhesive property and intensity are provided; and the application range is wide, and the material can be solidified in air, water oil or humid environment.
Description
Technical field
The invention belongs to technical field prepared by material.Be specifically related to a kind ofly take epoxy resin as base-material, and the bi-component epoxide-resin plugging material that contains degradable substance.
Background technology
The fast development of world economy, the energy in short supply, energy problem has been major issue urgently to be resolved hurrily.Therefore exploitation and searching new forms of energy are challenges that the whole world faces.Very abundant through verifying the deposit of whole world resinous shale, like this, the substitute that producing oil shale becomes oil is the direction that make great efforts countries in the world.
It is different that current various countries oil shale in-situ is exploited material water-proof material used, in this field original position exploitation, it is more successfully underground retoring (ICP) technology of Shell Co. Ltd, the material of control underground water used is to form freezing wall with liquefied ammonia, the method not only cost is high, and A leak of liquefied ammonia easily occurs and contaminate environment.Use for reference the shutoff method of Oil extraction, the degradable control underground water plugging material that this research intend to adopt high molecular polymer and inorganic materials, degradable high polymer material etc. (comprise natural and synthesize) to be used in conjunction with, at underground formation enclosed space, prevent that local water from flowing into mining area or oil, gas product overflows and affect production efficiency.
Effective water blockoff or the profile control and water plugging of Oilfield using are of a great variety.By technique, can be divided into single-fluid process plugging agent and two-fluid process plugging agent; By form, can be divided into gel-type, gel-type, sedimentation type and aqueous colloidal dispersion type; By severe condition, can be divided into high temperature, macropore, low permeability layer, high salinity ground stratotype etc.; According to purposes, can be divided into selective water shutoff agent and non-selective plugging agent.Because the object of the original position of resinous shale exploitation, product are different, control water plugging material used water shutoff material and the method used from oil production is different, and it also needs stifled oil except water blockoff, so can only select non-selective plugging material.Apply wider non-selective plugging material and have the materials such as epoxy resin, resol class.As everyone knows, epoxy resin is widely used in sealing material, but it is difficult to biological degradation.Be it at underground formation enclosed space, extract after shale oil, de-plugging difficulty, will cause underground water trickling not smooth like this, affects ground water circulation and balance.For this reason, guaranteeing, on the basis that this strength of materials requires, to add in right amount degradable substance, make it within the regular hour, degrade or dissolve, and in epoxy resin plugging material, form irregular holes, and recover trickling balance and the infiltration of underground water, reach the object of recover the original ecological balance.
Chinese patent CN101128503 prepared a kind of at least can bonding two kinds of faces or the bi-component reaction-type epoxy resin binder of parts, this tackiness agent can be connected to become the assembly that has fine anti-shearing, anti-collision and have the stability of some strength by vehicle part and oiliness metallic surface, and this assembly has good solidity to corrosion.Publication number is in the patent of CN101229662, to have proposed the bonding crushed marble of the high-intensity epoxy resin binder of a kind of use to become and have the decoration material of construction that aberration is little, intensity is high and turn waste into wealth.Patent CN101020807 has described a kind of epoxy resin adhesive for use in water, can construct under water, and sand-cement slurry, concrete and steel surface are all had to good applying property, its bond under water concrete mechanical property and bonding strength also higher.Patent CN1670109 has overcome the shortcomings such as general epoxy adhesive fragility is large, temperature tolerance is poor, prepared there is excellent oil resistant, the performance epoxy resin binder of water-fast, acidproof, alkaline-resisting, organic solvent-resistant.
Above-mentioned technical specification epoxy resin binder has good adhesiveproperties, mechanical property, and has good erosion resistance, but does not relate to the performance that makes material Partial digestion and dissolving.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the problem that in background technology, existing plugging material exists, provide a kind of can Partial digestion or the underground plugging material of dissolving.
Technical problem of the present invention solves by the following technical programs:
The underground plugging material of degradable, is comprised of A component and B component, wherein: A component comprises epoxy resin, toughner, thinner, coupling agent and filler; B component comprises solidifying agent, compound accelerant; It is characterized in that in A component, also having solvable or degradable substance A, or in B component, also have solvable or degradable substance B.
Each composition in A component is counted by weight, and its proportionlity is: 0～10 part of 100 parts of epoxy resin, 30～50 parts of toughner, 37～45 parts of reactive thinners, 2～7 parts of coupling agents, 0～100 part of filler, solvable or degradable substance A; Each composition in B component is counted by weight, and its proportionlity is: 25～30 parts, solidifying agent, 8～16 parts of compound accelerants; 0～10 part of solvable or degradable substance B; When wherein solvable or degradable substance A is different with solvable or degradable substance B, be 0; Also can use simultaneously.During use, by weight 1:0.15～0.35, mix A component and B component.
Described epoxy resin can be bisphenol A type epoxy resin, preferably bisphenol A type epoxy resin E-44 or E-51; The preferred reactive thinner of described thinner, preferably butylglycidyl ether; Described toughner can be rubber, polyethers, polysulfones, polyimide, nano silicon or nano-calcium carbonate, preferably thiorubber or polyimide; Described coupling agent can be organosilicon alkanes or non-silicane, preferred organic silicane γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (KH560) or 3-aminopropyl triethoxysilane (KH550); Described filler can be cement, silicon-dioxide or aluminum oxide, preferably cement; Described solidifying agent can be commercially available 810 underwater curing agent (production of Changsha chemical institute) or T31 solidifying agent (production of Shenyang City Xin Run resin institute), preferably 810 underwater curing agent; Described compound accelerant can be 2,4,6-tri-(dimethylamino methyl) phenol (DMP-30), diethylenetriamine (DETA), N, and one or more in N-dimethyl benzylamine (BDMA) etc., preferably by weight 1: 1～3 DMP-30 and DETA; Described solvable or degradable substance A can be carboxymethyl cellulose, starch, chitosan, polyvinyl alcohol, sodium alginate or sodium cellulosate, and solvable or degradable substance B can be polyacrylamide or poly(lactic acid).
The preparation method of the underground plugging material of a kind of degradable, first solvable or degradable substance A are dissolved or be distributed in epoxy resin (if consumption solvable or degradable substance A is 0 in A component, skip over this step), mix with toughner, reactive thinner, coupling agent, filler, stir, obtain A component; Solvable or degradable substance B is dissolved or be distributed in solidifying agent and (if consumption solvable or degradable substance B is 0 in B component, skip over this step), mix with compound accelerant, stir, obtain B component; A component and B component are deposited respectively.
A using method for degradable plugging material, by A component and 1: 0.15～0.35 mixing by weight of B component, stirs, and is needing the position of shutoff to solidify shutoff.
The underground plugging material of a kind of degradable of the present invention has following beneficial effect:
1,, after using certain time limit (18～24 months), meeting part automatic dissolving or dissolving, be conducive to environmental protection.
2, there is nonselective adhesiveproperties and intensity.
3, have wide range of applications, two-pack plugging material provided by the present invention is all curable in air, water, oil and wet environment.
Embodiment
The present invention is the underground plugging material of a kind of degradable environment-friendly type two-pack, by A component and B component, formed, wherein A component is the salient features important component part that determines this material, and directly impact is to the mechanical property of institute's plugging material, environmental performance, insulating property and corrosion resistance nature etc.Main component is bisphenol A type epoxy resin, and appropriate thinner, toughner, coupling agent, filler, solvable or degradable substance A etc.; B component is mainly curing agent composition, can make A component become tough and tensile solid or thermoset state from the thermoplasticity state-transition of liquid, thereby make material have certain physical strength and stability, main component is underwater curing agent, compound accelerant, solvable or degradable substance B etc.According to similarly mixing, microorganism is to mass degradation effect, interaction between substances principle, solvable or degradable substance A or B can make prepared plugging material use certain hour with rear section degraded or dissolve automatically.
Following embodiment further illustrates of the present invention, but does not limit the scope of the invention.
In following examples, tensile strength, elongation at break are pressed GB/T1040-1992 execution.Degradable substance is because of different in kind, and degradability parameter is different, and the measuring method of employing is different.Take embodiment 2 as example, the present invention adopt simple and convenient viscosimetry (Luo Yi, Tang Heqing, rice fine jade. Chinese plumbing, 2004,20 (3), 97; Mu Jingwen, Luo Yi, Tang and clear etc., Treatment of Industrial Water, 2006,26 (3), 77-79) measure the stripping quantity of polyacrylamide different time in differing temps water, while determining 100 ℃ by graphing method, dissolution rate is 5.575 * 10
-6g/mlh, in the time of 80 ℃, dissolution rate is 1.239 * 10
-6g/mlh.According to document (Tang Kangtai, Zhang Zicheng. oilfield chemistry, 1989,6 (1), 6-11) between the dissolution rate of described polyacrylamide and temperature, meet following relationship:
V=v
0exp(E
S/RT)
E wherein
sfor dissolution activation energy, v
0for constant.By calculating: the activation energy of polyacrylamide used
sbe 82.324 kcal/mol.
Calculate that thus prepared material is under 20 ℃ of conditions, 18～24 months degradables or dissolve more than 60%.In addition, by boiling weight-loss method, above-mentioned materials after soon solidifying is put into 65 ℃ of vacuum drying ovens and is dried to constant weight, accurately weigh its quality, then different time refluxes it in boiling water, after taking-up, put into vacuum drying oven and be dried under the same conditions constant weight, more accurately claim its quality, calculate that it is of poor quality.Method is calculated degraded or the dissolution time of degradable in this material or dissolved material thus, and to record result basically identical with viscosimetry.
Embodiment 1(comparative example):
Each component select materials and usage ratio in Table 1.
Table 1
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 1, after stirring, obtain A component.
2) preparation of B component: add 810 underwater curing agent and compound accelerants by listed part by weight in table 1 in another reactor, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.25 by weight, stir, obtain the underground plugging material of environmental protection.At room temperature solidify, the tensile strength after solidifying is completely 17.8MPa, elongation at break 7%, non-degradable or dissolving.
Embodiment 2:
Each component select materials and usage ratio in Table 2.
Table 2
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 2, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in 810 underwater curing agent in another reactor by the listed part by weight of table 2, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.25 by weight, stir, obtain the underground plugging material of environmental protection.Under room temperature, in water, solidify, the tensile strength after solidifying is completely 18.6MPa, the degradation rate >60% of 7%, 2 year polyacrylamide of elongation at break.
Embodiment 3:
Each component select materials and usage ratio in Table 3.
Table 3
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 3, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in T31 solidifying agent in another reactor by the listed part by weight of table 3, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.15 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 21.3MPa, and the elongation at break degradation rate of 5%, 2 year is >65%.
Embodiment 4:
Each component select materials and usage ratio in Table 4.
Table 4
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 4, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in 810 underwater curing agent in another reactor by the listed part by weight of table 4, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 18.1MPa, the elongation at break degradation rate >60% of 6%, 2 year.
Embodiment 5:
Each component select materials and usage ratio in Table 5.
Table 5
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 5, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in 810 underwater curing agent in another reactor by the listed part by weight of table 5, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.22 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 17.9MPa, and the elongation at break degradation rate of 7%, 2 year is >70%.
Embodiment 6:
Each component select materials and usage ratio in Table 6.
Table 6
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 6, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in T31 solidifying agent in another reactor by the listed part by weight of table 6, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.35 by weight, stir, obtain the underground plugging material of environmental protection.Under room temperature, in gasoline, solidify, the tensile strength after solidifying is completely 14.9MPa, the elongation at break degradation rate >50% of 8%, 2 year.
Embodiment 7:
Each component select materials and usage ratio in Table 7.
Table 7
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 7, after stirring, obtain component A.
2) preparation of B component: polyacrylamide is dissolved in 810 underwater curing agent in another reactor by the listed part by weight of table 7, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.Under room temperature, in air set, the tensile strength after solidifying is completely 19.7MPa, the elongation at break degradation rate >60% of 6%, 2 year.
Embodiment 8:
Each component select materials and usage ratio in Table 8.
Table 8
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 8, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in T31 solidifying agent in another reactor by the listed part by weight of table 8, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 20.7MPa, the elongation at break degradation rate >60% of 4%, 2 year.
Embodiment 9:
Each component select materials and usage ratio in Table 9.
Table 9
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 9, after stirring, obtain A component.
2) preparation of B component: poly(lactic acid) is dissolved in 810 underwater curing agent in another reactor by the listed part by weight of table 9, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 21.4MPa, the elongation at break degradation rate >60% of 7%, 2 year.
Embodiment 10:
Each component select materials and usage ratio in Table 10.
Table 10
Preparation and application is as follows:
1) preparation of A component: in reactor, Zulkovsky starch is scattered in to butylglycidyl ether by the listed part by weight of table 10, then adds all the other each compositions in the listed A component of table 10, after stirring, obtain A component.
2) preparation of B component: add each composition of B component by the listed part by weight of table 10 in another reactor, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 21.3MPa, the elongation at break degradation rate >60% of 6%, 2 year.
Embodiment 11:
Each component select materials and usage ratio in Table 11.
Table 11
Preparation and application is as follows:
1) preparation of A component: in reactor, chitosan is scattered in to butylglycidyl ether by the listed part by weight of table 11, then adds all the other each compositions in the listed A component of table 11, after stirring, obtain A component.
2) preparation of B component: add each composition of B component by the listed part by weight of table 11 in another reactor, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 18.1MPa, the elongation at break degradation rate >60% of 7%, 2 year.
Embodiment 12:
Each component select materials and usage ratio in Table 12.
Table 12
Preparation and application is as follows:
1) preparation of A component: in reactor, sodium alginate is scattered in to butylglycidyl ether by the listed part by weight of table 12, then adds all the other each compositions in the listed A component of table 12, after stirring, obtain A component.
2) preparation of B component: add each composition of B component by the listed part by weight of table 12 in another reactor, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.At room temperature solidify, the tensile strength after solidifying is completely 17.4MPa, the elongation at break degradation rate >60% of 7%, 2 year.
Embodiment 13:
Each component select materials and usage ratio in Table 13.
Table 13
Preparation and application is as follows:
1) preparation of A component: in reactor, sodium cellulosate is scattered in to butylglycidyl ether by the listed part by weight of table 13, then adds all the other each compositions in the listed A component of table 13, after stirring, obtain A component.
2) preparation of B component: add each composition of B component by the listed part by weight of table 13 in another reactor, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.At room temperature solidify, the tensile strength after solidifying is completely 16.9MPa, the elongation at break degradation rate >60% of 7%, 2 year.
Embodiment 14:
Each component select materials and usage ratio in Table 14.
Table 14
Preparation and application is as follows:
1) preparation of A component: each composition in A component is added in reactor by the listed part by weight of table 14, after stirring, obtain A component.
2) preparation of B component: polyacrylamide is dissolved in 810 underwater curing agent at another reactor by the listed part by weight of table 14, then adds compound accelerant, after stirring, obtain B component.
3) while using, by the A component making above and B component, be to mix at 1: 0.20 by weight, stir, obtain the underground plugging material of environmental protection.In wet environment, solidify, the tensile strength after solidifying is completely 20.6MPa, the elongation at break degradation rate >50% of 3%, 2 year.
Claims (6)
1. the underground plugging material of degradable, is comprised of A component and B component, wherein: A component comprises epoxy resin, toughner, thinner, coupling agent and filler; B component comprises solidifying agent, compound accelerant; It is characterized in that in A component, also having solvable or degradable substance A, or in B component, also have solvable or degradable substance B; Described toughner is thiorubber or polyimide; Described compound accelerant is 2,4,6-three (dimethylamino methyl) phenol and the diethylenetriamines by weight 1: 1～3; Described solvable or degradable substance A is carboxymethyl cellulose, starch, chitosan, polyvinyl alcohol, sodium alginate or sodium cellulosate, and solvable or degradable substance B is polyacrylamide or poly(lactic acid).
2. the underground plugging material of a kind of degradable according to claim 1, it is characterized in that, each composition in A component is counted by weight, and its proportionlity is: 100 parts of epoxy resin, 30～50 parts of toughner, 37～45 parts of thinners, 2～7 parts of coupling agents, 0～100 part of filler, solvable or degradable substance A0～10 part; Each composition in B component is counted by weight, and its proportionlity is: 25～30 parts, solidifying agent, 8～16 parts of compound accelerants; Solvable or degradable substance B0～10 part; When wherein solvable or degradable substance A is different with solvable or degradable substance B, be 0.
3. according to the underground plugging material of a kind of degradable described in claim 1 or 2 any one, it is characterized in that, described epoxy resin is bisphenol A type epoxy resin E-44 or E-51; Described thinner is butylglycidyl ether; Described coupling agent is organosilicon alkanes γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane or 3-aminopropyl triethoxysilane; Described filler is cement, silicon-dioxide or aluminum oxide; Described solidifying agent is 810 underwater curing agent or T31 solidifying agent.
4. the underground plugging material of a kind of degradable according to claim 3, is characterized in that described filler is cement.
5. a preparation method for the underground plugging material of degradable of claim 1, first dissolves solvable or degradable substance A or be distributed in epoxy resin, mixes with toughner, thinner, coupling agent, filler, stirs, and obtains A component; Solvable or degradable substance B dissolved or be distributed in solidifying agent, mix with compound accelerant, stirring, obtaining B component.
6. a using method for the underground plugging material of degradable of claim 1, by A component and 1: 0.15～0.35 mixing by weight of B component, stirs, and is needing the position of shutoff to solidify shutoff.
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| CN201210548442.0A CN103013052B (en) | 2012-12-17 | 2012-12-17 | Degradable underground blocking material |
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| CN201210548442.0A CN103013052B (en) | 2012-12-17 | 2012-12-17 | Degradable underground blocking material |
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| CN102153977B (en) * | 2011-03-11 | 2013-11-06 | 中南林业科技大学 | Anti-seepage leak-stopping epoxy adhesive and preparation method thereof |
| CN102504670A (en) * | 2011-10-27 | 2012-06-20 | 北京东方雨虹防水技术股份有限公司 | Permeable epoxy resin waterproof coating for concrete |
| CN102653673B (en) * | 2012-01-05 | 2014-05-14 | 中国石油天然气股份有限公司 | Biodegradable temporary plugging additive |
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2012
- 2012-12-17 CN CN201210548442.0A patent/CN103013052B/en active Active
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