CN115725283A - Lignin-based composite channeling sealing agent and preparation method and application thereof - Google Patents
Lignin-based composite channeling sealing agent and preparation method and application thereof Download PDFInfo
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- CN115725283A CN115725283A CN202111009358.7A CN202111009358A CN115725283A CN 115725283 A CN115725283 A CN 115725283A CN 202111009358 A CN202111009358 A CN 202111009358A CN 115725283 A CN115725283 A CN 115725283A
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- lignin
- agent
- based composite
- sealing agent
- channeling sealing
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- 230000005465 channeling Effects 0.000 title claims abstract description 96
- 229920005610 lignin Polymers 0.000 title claims abstract description 93
- 238000007789 sealing Methods 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 92
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002562 thickening agent Substances 0.000 claims abstract description 27
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- 239000000295 fuel oil Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 28
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000003513 alkali Substances 0.000 claims description 15
- 229920000459 Nitrile rubber Polymers 0.000 claims description 13
- 150000001408 amides Chemical group 0.000 claims description 13
- 230000033558 biomineral tissue development Effects 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 239000000440 bentonite Substances 0.000 claims description 12
- 229910000278 bentonite Inorganic materials 0.000 claims description 12
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 150000001299 aldehydes Chemical class 0.000 claims description 7
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims description 3
- 235000010350 erythorbic acid Nutrition 0.000 claims description 3
- 229940026239 isoascorbic acid Drugs 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 230000002255 enzymatic effect Effects 0.000 claims description 2
- 238000004880 explosion Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 238000005292 vacuum distillation Methods 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 230000000903 blocking effect Effects 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 238000010276 construction Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 27
- 239000000499 gel Substances 0.000 description 24
- 230000018044 dehydration Effects 0.000 description 20
- 238000006297 dehydration reaction Methods 0.000 description 20
- 238000012360 testing method Methods 0.000 description 17
- 239000000084 colloidal system Substances 0.000 description 16
- 239000003292 glue Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 235000011121 sodium hydroxide Nutrition 0.000 description 8
- 239000004973 liquid crystal related substance Substances 0.000 description 7
- 239000005011 phenolic resin Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000011435 rock Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000007071 enzymatic hydrolysis Effects 0.000 description 5
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 5
- 238000009830 intercalation Methods 0.000 description 5
- 150000002989 phenols Chemical class 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 230000002687 intercalation Effects 0.000 description 4
- 235000015110 jellies Nutrition 0.000 description 4
- 239000008274 jelly Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- -1 phenolic aldehyde Chemical class 0.000 description 3
- 229920001568 phenolic resin Polymers 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 3
- 239000004971 Cross linker Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229920001732 Lignosulfonate Polymers 0.000 description 2
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- CXRFDZFCGOPDTD-UHFFFAOYSA-M Cetrimide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)C CXRFDZFCGOPDTD-UHFFFAOYSA-M 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229920005551 calcium lignosulfonate Polymers 0.000 description 1
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 description 1
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- Sealing Material Composition (AREA)
Abstract
The invention provides a lignin-based composite channeling sealing agent and a preparation method and application thereof. The lignin-based composite channeling sealing agent comprises lignin, a modified cross-linking agent, a thickening agent, a stabilizing agent and prepared water. Adding the thickening agent into prepared water for full dissolution, then adding lignin and a stabilizing agent, and uniformly mixing to obtain a mixed solution; and (3) dripping a modified cross-linking agent into the mixed solution, uniformly mixing, and then adjusting the pH value to obtain the lignin-based composite channeling sealing agent. The lignin-based composite channeling sealing agent disclosed by the invention has the advantages that the blocking strength, toughness, blocking efficiency, effective period and the like of a lignin-based channeling sealing system are obviously improved through the modification of the cross-linking agent, the blocking rate is higher than 99.05%, a steam channeling channel can be effectively blocked for a long time, the high-efficiency development of a heavy oil reservoir is realized, the requirements on the performance and the economy of field construction are met, and the practicability is higher.
Description
Technical Field
The invention relates to the technical field of oil field chemicals, in particular to a lignin-based composite channeling sealing agent and a preparation method and application thereof.
Background
In the process of thick oil steam exploitation, after high-frequency steam stimulation, steam channeling channels can be generated in the stratum, so that steam channeling interference among wells is caused, the exploitation effect is poor, and therefore a high-efficiency blocking steam channeling technology needs to be reserved.
There are several methods for thick oil seal steam channeling and for inhibiting side water intrusion, but some drawbacks are common. At present, channeling sealing agents commonly used in oil fields mainly comprise high-temperature jelly, foam, solid-phase particle plugging agents and the like, wherein solid-phase particles are easy to be retained in a near-wellbore area, foam is heavy in profile control, and the plugging effect is poor. The high-temperature jelly is widely applied, the gelling agent of the high-temperature jelly mainly comprises lignin, tannin extract, humic acid and other rigid polymers, wherein the temperature resistance of the plugging agent taking the lignin as the main agent is good and the strength is high after the cross-linking reaction, and the material has wide sources and relatively low price.
On the one hand, however, the lignin has high methoxyl content, low hydroxyl content, large steric hindrance and obviously insufficient reaction activity; on the other hand, because of a large number of benzene ring groups in the structure of the phenolic resin, the channeling sealing agent prepared by taking the benzene ring groups as the cross-linking agent has poor toughness and short effective period, and the application of the phenolic resin cross-linking agent in the future heavy oil thermal recovery plugging operation is limited.
Therefore, the 'lignin-phenolic aldehyde' channeling sealing agent has the problems of large using amount of lignin and a cross-linking agent, low colloid strength and poor toughness. When the external force exceeds the strength of the colloid, the colloid is broken, and the system cannot recover, so that the channeling sealing performance is greatly lost.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a lignin-based composite channeling sealing agent and a preparation method and application thereof. The viscosity of the lignin-based composite channeling sealing agent at normal temperature (25 ℃) is 8.4-17.8mPa & s, and the lignin-based composite channeling sealing agent has good pumpability; the glue can be controlled within a wider temperature range (90-300 ℃) for 2-168h, and the glue strength is more than 0.074-0.088 MPa; the gel is not broken at the high temperature of 300 ℃ for 60 days, the volume of the colloid is basically unchanged, and the dehydration rate is less than 3.3 percent; the plugging rate is higher than 99.05%, and the steam channeling channel can be effectively plugged for a long time, so that the high-efficiency development of the heavy oil reservoir is realized. Through the modification of the cross-linking agent, the blocking strength, the toughness, the blocking efficiency, the validity period and the like of the lignin-based channeling sealing system are obviously improved, the requirements on the performance and the economy of field construction are met, and the practicability is higher.
One of the purposes of the invention is to provide a lignin-based composite channeling sealing agent, which is prepared from the raw materials comprising the following components;
lignin, a modified cross-linking agent, a thickening agent, a stabilizing agent and preparation water;
based on the total weight of the raw materials as 100 percent,
the addition amount of the lignin is 3-9wt%;
the addition amount of the modified cross-linking agent is 0.1-3wt%;
the addition amount of the thickening agent is 0.001 to 0.15 weight percent;
the addition amount of the stabilizer is 0.001-0.05wt%.
In order to further obtain better effect, in particular, the channeling sealing agent can realize controllable crosslinking at higher gelling temperature, and the jelly strength is better, preferably,
based on the total weight of the raw materials as 100 percent,
the addition amount of the lignin is 5.5-7wt%;
the addition amount of the modified crosslinking agent is 0.5-2%, more preferably 1-1.8wt%;
the addition amount of the thickening agent is 0.05-0.1wt%;
the addition amount of the stabilizer is 0.01-0.03wt%.
In the present invention, the amount of water to be added is suitably formulated so that the above components are within the above-mentioned range, and the skilled person can determine the amount according to the actual situation.
Preferably, the first and second liquid crystal materials are,
the lignin is at least one selected from alkali lignin, enzymolysis lignin, sodium lignosulfonate, chlorinated lignin, steam explosion lignin, ground wood lignin or sulfur lignin; preferably at least one selected from alkali lignin or enzymatic lignin;
in the present invention, lignosulfonate is lignosulfonate commonly used in the art, including but not limited to sodium lignosulfonate, calcium lignosulfonate, and the like.
The thickener is an amide thickener, preferably at least one of acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer (AM-AMPS copolymer), and has the weight average molecular weight of 500-3000 ten thousand; preferably 1000 to 2000 ten thousand.
Preferably, the first and second liquid crystal materials are,
the stabilizer is selected from at least one of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium dithionite, isoascorbic acid or thiourea; and/or
In the present invention, the prepared water is not particularly limited, and may be a river, a lake, sea water, ground water, artificial water, oilfield produced water, or the like, and is preferably water having a mineralization degree of less than 200000mg/L, and more preferably water having a mineralization degree of less than 100000 mg/L.
Preferably, the first and second liquid crystal materials are,
the preparation method of the modified cross-linking agent comprises the following steps:
premixing water, phenol, aldehyde, nitrile rubber and organic bentonite, adding an alkali catalyst, and heating for reaction; after the reaction is finished, adjusting the pH value, and distilling to obtain the modified crosslinking agent.
Preferably, the first and second liquid crystal materials are,
the phenol is selected from at least one of phenol, hydroquinone, resorcinol or catechol; and/or
The aldehyde is selected from at least one of formaldehyde, acetaldehyde or furfural; and/or
The nitrile rubber is selected from liquid nitrile rubber, more preferably at least one of LNBR-26 and LNBR-40; and/or
In the invention, the organic bentonite is the organic bentonite commonly used in the prior art, and the preferred self-intercalation agent is at least one organic bentonite of octadecyl trimethyl ammonium chloride, octadecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide and tetradecyl trimethyl ammonium chloride;
the alkali catalyst is soluble alkali, preferably at least one of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate or sodium bicarbonate.
Preferably, the first and second liquid crystal materials are,
the mass ratio of the phenol to the aldehyde to the nitrile rubber is 1: (1.5-4): (0.01-0.05); preferably 1: (1.6-3): (0.02-0.04);
the concentration of the phenol is 1.5-3wt%;
the concentration of the organic bentonite is 0.5-2.5wt%;
the concentration of the alkali catalyst is 0.5-1wt%;
the pH value is adjusted to 7.5-9.5.
In the present invention, the conditions for the reaction of the modifying crosslinking agent are not particularly limited, and the reaction may be completed; the stirring speed in each step is not particularly limited, and the pH adjustment is also a substance commonly used in the art for adjusting pH, such as dilute hydrochloric acid, dilute sulfuric acid, and the like, for achieving the object and uniformly mixing.
Preferably, the first and second liquid crystal materials are,
the stirring speed of the premixing is 150-300 r/min;
the heating reaction temperature is 78-88 ℃, and the reaction time is 30-90min;
the distillation mode is vacuum distillation; distilling until the solid content is more than or equal to 40 percent.
In the invention, the lignin, the thickening agent, the preparation raw material of the modified cross-linking agent and the stabilizing agent can be obtained commercially.
The inventor of the invention unexpectedly discovers in research that the lignin-phenolic aldehyde sealing channeling system has poor strength and insufficient toughness after being gelled, and when external force exceeds the strength of colloid, the colloid is crushed, and the system cannot be recovered, so that the sealing channeling performance is greatly lost. The C-C bond of the nitrile rubber has strong space rotation deformability, and the C-N bond can be hydrolyzed at high temperature to form an amido bond so as to react with the phenolic aldehyde. By introducing the nitrile rubber into the phenolic aldehyde, the space network structure of the lignin can be intertwined and reinforced, and the colloid strength and toughness after gelling are improved. Meanwhile, bentonite is required to be introduced into phenolic aldehyde for modification, and the bentonite can be uniformly dispersed in a gelling liquid system to avoid agglomeration, so that the nano reinforcing filler has the effect of improving the strength of the plugging agent obtained by gelling the cross-linking agent; the lignin-based plugging agent can interact with lignin, so that the toughness of the lignin-based plugging agent is improved, and the plugging performance is improved. The lignin-based composite channeling sealing agent is matched with other components for use, has viscosity of 8.4-17.8mPa & s at normal temperature (25 ℃), and has good pumpability; the glue can be controlled within a wider temperature range (90-300 ℃) for 2-168h, and the glue strength is more than 0.074-0.088 MPa; the gel is not broken at the high temperature of 300 ℃ for 60 days, the volume of the colloid is basically unchanged, and the dehydration rate is less than 3.3 percent; the plugging rate is higher than 99.05%, and the steam channeling channel can be effectively plugged for a long time, so that the high-efficiency development of the heavy oil reservoir is realized.
The other purpose of the invention is to provide a preparation method of the lignin-based composite channeling sealing agent, which comprises the following steps:
(1) Adding the thickening agent into prepared water for full dissolution, then adding lignin and a stabilizing agent, and uniformly mixing to prepare a mixed solution;
(2) And (3) dripping a modified cross-linking agent into the mixed solution, uniformly mixing, and then adjusting the pH value to obtain the lignin-based composite channeling sealing agent.
Preferably, the first and second liquid crystal materials are,
in step (2), the pH is adjusted to 8 to 11, preferably 9 to 10.
In the invention, whether the pH value needs to be adjusted or not is determined according to the pH value of the channeling sealing system; if the pH value of the channeling sealing system is within the above range, the pH value may not be adjusted.
The pH regulator used for regulating the pH value can be acid and alkaline substances which are commonly used in the prior art for regulating the pH value; preferably, the pH adjusting agent is at least one selected from the group consisting of dilute hydrochloric acid, dilute sulfuric acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium acetate, and ammonia water.
In the present invention, the specific substance and amount of the added pH adjuster may be selected and adjusted according to the acid and alkali conditions of the channeling-sealing system, so that the pH value in the channeling-sealing system is within the above-defined pH range.
Preferably, the content of the pH regulator is 0.1-1.5wt% based on the total weight of the raw materials as 100%; more preferably, the content of the pH regulator is 0.5 to 1.2wt%.
In the present invention, the stirring speed is not particularly limited, and it is assumed that the lignin-based composite channeling sealing agent can be uniformly mixed.
The invention also provides the application of the lignin-based composite channeling sealing agent in heavy oil exploitation.
Compared with the prior art, the invention has the following advantages:
the viscosity of the lignin-based composite channeling sealing agent at normal temperature (25 ℃) is 8.4-17.8mPa & s, and the lignin-based composite channeling sealing agent has good pumpability; the glue (2-168 h) can be controlled in a wider temperature range (90-300 ℃), and the glue strength is more than 0.074-0.088 MPa; the gel is not broken at the high temperature of 300 ℃ for 60 days, the volume of the colloid is basically unchanged, and the dehydration rate is less than 3.3 percent; the plugging rate is higher than 99.05%, and the steam channeling channel can be effectively plugged for a long time, so that the high-efficiency development of the heavy oil reservoir is realized.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The raw material sources are as follows:
the enzymatic hydrolysis lignin is purchased from Shandong Longli Biotechnology GmbH, and has an effective content of 94.8wt%.
Sodium lignosulfonate, alkali lignin were purchased from carbofuran technologies ltd.
The amide thickener (AM-AMPS copolymer) is purchased from Shandong Baomo biological chemical industry Co., ltd, has an effective content of about 88wt%, and has a weight average molecular weight of 1500 ten thousand.
The phenolic resin is purchased from Shandong Dongynghaoyu chemical industry Co., ltd, and the effective content is about 50wt%.
Liquid nitrile rubber was purchased from petroleum lanzhou petrochemical division.
Phenols, aldehydes, stabilizers were purchased from carbofuran technologies ltd.
Organobentonite was purchased from Zhejiang Fenghong New materials, inc.
The test method comprises the following steps:
initial viscosity measurement:
the viscosity was measured using a Brookfield DV-III viscometer.
And (3) testing the colloid strength:
the colloid strength is tested by adopting a breakthrough vacuum degree method, and the specific operation is as follows: and (3) filling the gelled colloid into a test bottle of a breakthrough vacuum degree experimental device, inserting a 1mL pipette tip part into a position 1cm below the surface of the colloid, starting a vacuum pump, slowly adjusting a knob to increase the vacuum degree of the system, when air breaks through the colloid, repeatedly measuring each sample for 3 times, and taking the arithmetic mean value of the samples as the final strength value.
And (3) testing the plugging rate:
filling a simulated rock core (the diameter of the rock core is 25mm, the length of the rock core is 600 mm), vacuumizing and saturating with water. Firstly, injecting water into a rock core at a certain flow rate, and measuring the permeability (k) of the rock core before plugging 0 ) (ii) a Then injecting different plugging agents into the rock core at the injection rate of 2mL/min under the condition of gas-liquid ratio 1:1 for stabilizing (forming)Glue), heating the heating sleeve to a specified temperature, and performing subsequent displacement phase displacement; and finally, water injection is carried out to measure the permeability (k') after the core is plugged. The plugging rate is taken as a parameter for representing the plugging effect of the plugging agent, and the calculation formula of the plugging rate is
Wherein k is 0 Permeability before plugging, μm 2 (ii) a k' is the post-occlusion permeability, μm 2 。
The heating temperature of the heating jacket corresponds to the temperature required by the displacement phase to be simulated, and the displacement phase to be simulated can be water or water vapor.
The dehydration rate test method comprises the following steps:
after the reaction of the reactor is carried out by a 300 ℃ high-temperature stability test, the volume of free water outside the colloid in the reactor is measured, the dehydration rate is the ratio of the volume of the free water to the total volume of the colloid-forming liquid, and the volume is a numerical value measured at room temperature.
Preparation example 1
Preparation of modified Cross-linker FQ-1
(1) Adding 87.55g water, 2.5g phenol, 7.5g formaldehyde, 0.1g LNBR-26, 1.6g organobentonite (cetyl trimethyl ammonium chloride as intercalation agent) into a three-neck flask equipped with a stirrer and a reflux pipe, stirring uniformly at 250 r/min, and finishing premixing;
(2) Then the temperature of the system is raised to the set temperature of 80 ℃, 0.75g of NaOH is added under stirring, stirring is continued, heating and reflux are carried out, and the reaction lasts for 40min;
(3) After the reaction is finished, adjusting the pH value to 7.5, and distilling under reduced pressure until the solid content is 55% to obtain the modified cross-linking agent FQ-1.
Preparation example 2
Preparation of modified Cross-linker FQ-2
(1) Adding 92.255g water, 1.8g hydroquinone, 4.2g acetaldehyde, 0.045g LNBR-40 (liquid nitrile butadiene rubber 40) and 1g organic bentonite (tetradecyltrimethyl ammonium chloride is used as an intercalation agent) into a three-neck flask provided with a stirrer and a return pipe, uniformly stirring at the speed of 250 revolutions per minute, and finishing premixing;
(2) Then the temperature of the system is raised to the set temperature of 80 ℃, 0.7g of potassium hydroxide is added under stirring, the stirring is continued at 700 r/min, and the heating, the reflux and the reaction are carried out for 80min;
(3) After the reaction is finished, adjusting the pH value to 8.0, and distilling under reduced pressure until the solid content is 48% to obtain the modified cross-linking agent FQ-2.
Preparation example 3
The preparation of the modified cross-linking agent FQ-3 comprises the following steps:
(1) Adding 91.988g water, 2.1g phenol, 3.8g formaldehyde, 0.052g LNBR-26 (liquid nitrile rubber 26) and 1.2g organic bentonite (octadecyl trimethyl ammonium chloride is used as an intercalation agent) into a three-neck flask provided with a stirrer and a return pipe, uniformly stirring at the speed of 250 revolutions per minute, and finishing premixing;
(2) Then the temperature of the system is raised to 85 ℃, 0.86g of NaOH is added under stirring, the stirring is continued at 700 r/min, and the heating, the reflux and the reaction are carried out for 60min;
(3) After the reaction is finished, adjusting the pH value to 9.0, and distilling under reduced pressure until the solid content is 51% to obtain the modified cross-linking agent FQ-3.
Example 1
Dissolving 0.08g of amide thickening agent (AM-AMPS copolymer) in 80g of prepared water with the mineralization degree of 15000mg/L, and stirring at the rotating speed of 500r/min until the amide thickening agent is uniformly dissolved; then 6.4g of enzymatic hydrolysis lignin and 0.025g of sodium thiosulfate are added; after uniformly stirring, slowly dropping 1.7g of modified cross-linking agent FQ-1, adding NaOH to adjust the pH value to 9.5, adding prepared water with the degree of mineralization of 15000mg/L to the fixed quantity of 100g, and uniformly stirring to obtain the lignin-based composite channeling sealing agent. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 13.2mPa & s; the strength of the gel reaches 0.084MPa after the gel is formed at the temperature of 100 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 1.8 percent; and (3) performing plugging test on the obtained channeling sealing agent, wherein the plugging rate is 99.58%.
Example 2
Dissolving 0.05g of amide thickener (AM-AMPS copolymer) in 80g of prepared water with the mineralization degree of 20000mg/L, and stirring at the rotation speed of 500r/min until the amide thickener is uniformly dissolved; then adding 5.5g of enzymatic hydrolysis lignin and 0.01g of thiourea; after uniformly stirring, slowly dripping 1g of modified cross-linking agent FQ-1, adding NaOH to adjust the pH value to 10, adding a certain amount of preparation water with the mineralization degree of 20000mg/L to 100g, and uniformly stirring to obtain the lignin-based composite channeling sealing agent. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 8.4mPa & s; the strength of the gel reaches 0.074MPa after the gel is formed at the temperature of 150 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 2.4 percent; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 99.11%.
Example 3
Dissolving 0.06g of amide thickener (AM-AMPS copolymer) in 80g of prepared water with the mineralization degree of 50000mg/L, and stirring at the rotating speed of 500r/min until the amide thickener is uniformly dissolved; then 6.6g of enzymatic hydrolysis lignin and 0.028 thiourea are added; after uniformly stirring, slowly dripping 1.6g of modified cross-linking agent FQ-2, adding NaOH to adjust the pH value to 9.5, adding a fixed amount of prepared water with the mineralization degree of 50000mg/L to 100g, and uniformly stirring to obtain the lignin-based composite channeling sealing agent. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 9.0mPa & s; the strength of the gel reaches 0.079MPa after the gel is formed at 180 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 1.9 percent; and the plugging rate of the obtained channeling sealing agent is 99.36 percent by a plugging test. The lignin-based composite channeling sealing agent has the strength of 0.076MPa after being gelled at the temperature of 300 ℃.
Example 4
Dissolving 0.1g of amide thickener (AM-AMPS copolymer) in 80g of prepared water with the mineralization degree of 80000mg/L, and stirring at the rotation speed of 500r/min until the amide thickener is uniformly dissolved; then adding 7g of enzymatic hydrolysis lignin and 0.01g of isoascorbic acid; after stirring uniformly, slowly dropping 1.8g of modified cross-linking agent FQ-2, adding NaOH to adjust the pH value to 9, adding prepared water with the mineralization degree of 80000mg/L to a fixed quantity of 100g, and stirring uniformly to obtain the lignin-based composite channeling sealing agent. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 17.8mPa & s; the strength of the gel reaches 0.088MPa after the gel is formed at the temperature of 120 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 1.1%; and (3) performing plugging test on the obtained channeling sealing agent, wherein the plugging rate is 99.58%.
Example 5
Dissolving 0.07g of amide thickening agent (AM-AMPS copolymer) in 80g of prepared water with the mineralization degree of 80000mg/L, and stirring at the rotating speed of 500r/min until the amide thickening agent is uniformly dissolved; then 4g of alkali lignin and 0.015g of sodium hydrosulfite are added; after stirring evenly, 0.5g of modified cross-linking agent FQ-2 is slowly dropped, naOH is added to adjust the pH value to 9.5, then the prepared water with the mineralization degree of 80000mg/L is added to quantify to 100g, and the lignin-based composite channeling sealing agent is obtained after stirring evenly. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 10.2mPa & s; the strength of the gel reaches 0.075MPa after the gel is formed at the temperature of 120 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 2.9 percent; and (3) performing plugging test on the obtained channeling sealing agent, wherein the plugging rate is 99.09%.
Example 6
The preparation method of the embodiment 6 is the same as that of the embodiment 1, except that the lignin is sodium lignosulfonate, and the modified cross-linking agent is FQ-3, so that the lignin-based composite channeling sealing agent is obtained. The initial viscosity of the lignin-based composite channeling sealing agent at 25 ℃ is 17.1mPa & s; the strength of the gel reaches 0.074MPa after the gel is formed at the temperature of 100 ℃; the glue is not broken after being kept for 60 days at 300 ℃, and the dehydration rate is 3.3 percent; and (3) performing plugging test on the obtained channeling sealing agent, wherein the plugging rate is 99.05%.
Comparative example 1
An experiment was conducted in the same manner as in example 1 except that the modified crosslinking agent FQ-1 was replaced with an unmodified phenol resin to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 11.4mPa & s; the strength after gelling is 0.039MPa at 100 ℃, the gel is broken and the dehydration rate is 41.4 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 83.99%.
Comparative example 2
An experiment was conducted in the same manner as in example 2 except that the modified crosslinking agent FQ-1 was replaced with an unmodified phenol resin to obtain a channeling agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 7.1mPa & s; the strength after gelling is 0.032MPa at 150 ℃, the gel is broken and the dehydration rate is 37.1 percent after 60 days at 300 ℃; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 78.56%.
Comparative example 3
An experiment was conducted in the same manner as in example 3 except that the modified crosslinking agent FQ-2 was replaced with an unmodified phenol resin to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 7.2mPa & s; the strength after gelling is 0.035MPa at 180 ℃, the gel is broken and the dehydration rate is 43.1 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 80.03%.
Comparative example 4
An experiment was conducted in the same manner as in example 4 except that the modified crosslinking agent FQ-2 was replaced with an unmodified phenol resin to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent is 15.3mPa & s at 25 ℃; the strength after gelling is 0.051MPa at 120 ℃, the gel is broken and the dehydration rate is 33.4 percent after 60 days at 300 ℃; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 84.16%.
Comparative example 5
Preparation of modified crosslinking agent FQ-4:
it was prepared in substantially the same manner as the crosslinking agent prepared in preparation example 2, except that the raw material for the modified crosslinking agent did not contain organobentonite.
An experiment was conducted in the same manner as in example 4 except that the modified crosslinking agent FQ-2 was replaced with the modified crosslinking agent FQ-4 to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 13.4mPa & s; the strength after gelling is 0.071MPa at 120 ℃, the gel is broken and the dehydration rate is 16.5 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 92.59%.
Comparative example 6
Preparation of modified crosslinking agent FQ-5:
the preparation method is basically the same as that of the crosslinking agent prepared in preparation example 2, except that the raw material of the modified crosslinking agent does not contain LNBR-40 (liquid nitrile rubber 40).
An experiment was conducted in the same manner as in example 4 except that the modified crosslinking agent FQ-2 was replaced with the modified crosslinking agent FQ-5 to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 12.1mPa & s; the strength after gelling is 0.078MPa at 120 ℃, and the gel is broken and the dehydration rate is 18.6 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 88.45%.
Comparative example 7
Preparation of modified crosslinking agent FQ-6:
the preparation method is basically the same as that of the cross-linking agent prepared in preparation example 2, except that the addition amount of LNBR-40 (liquid nitrile butadiene rubber 40) in the raw materials of the modified cross-linking agent is 0.845g, and the addition amount of water is 91.455g.
An experiment was conducted in the same manner as in example 4 except that the modified crosslinking agent FQ-2 was replaced with a modified crosslinking agent FQ-6 to obtain a channeling agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 16.1mPa & s; the strength after gelling is 0.080MPa at 120 ℃, and the gel is broken and the dehydration rate is 15.42 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 90.24%.
Comparative example 8
Preparation of modified crosslinking agent FQ-7:
the preparation method is basically the same as that of the cross-linking agent prepared in preparation example 2, except that the addition amount of the organic bentonite (tetradecyltrimethyl ammonium chloride is used as an intercalation agent) in the raw material of the modified cross-linking agent is 4.255g, and the addition amount of the water is 89g.
An experiment was conducted in the same manner as in example 4 except that the modified crosslinking agent FQ-2 was replaced with the modified crosslinking agent FQ-7 to obtain a channeling sealing agent. The initial viscosity of the channeling sealing agent at 25 ℃ is 13.1mPa & s; the strength after gelling is 0.075MPa at 120 ℃, the gel is broken and the dehydration rate is 10.9 percent at 300 ℃ for 60 days; and (3) performing a plugging test on the obtained channeling sealing agent, wherein the plugging rate is 93.21%.
As can be seen by comparing the examples and the comparative examples, the viscosity of the lignin-based composite channeling sealing agent is 8.4-17.8 mPa.s at normal temperature (25 ℃), and the lignin-based composite channeling sealing agent has good pumpability; the glue can be controlled within a wider temperature range (90-300 ℃) for 2-168h, and the glue strength is more than 0.074-0.088 MPa; the gel is not broken at the high temperature of 300 ℃ for 60 days, the volume of the colloid is basically unchanged, and the dehydration rate is less than 3.3 percent; the plugging rate is higher than 99.05%, and the steam channeling channel can be effectively plugged for a long time, so that the high-efficiency development of the heavy oil reservoir is realized.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. A lignin-based composite channeling sealing agent is characterized in that: the lignin-based composite channeling sealing agent is prepared from the following raw materials;
lignin, a modified cross-linking agent, a thickening agent, a stabilizing agent and prepared water;
based on the total weight of the raw materials as 100 percent,
the addition amount of the lignin is 3-9wt%;
the addition amount of the modified cross-linking agent is 0.1-3wt%;
the addition amount of the thickening agent is 0.001 to 0.15 weight percent;
the stabilizer is added in an amount of 0.001-0.05wt%.
2. The lignin-based composite channeling sealing agent according to claim 1, wherein:
based on the total weight of the raw materials as 100 percent,
the addition amount of the lignin is 5.5-7wt%;
the addition amount of the modified cross-linking agent is 1-1.8wt%;
the addition amount of the thickening agent is 0.05-0.1wt%;
the addition amount of the stabilizer is 0.01-0.03wt%.
3. The lignin-based composite channeling sealing agent according to claim 1, wherein:
the lignin is at least one selected from alkali lignin, enzymolysis lignin, sodium lignosulfonate, chlorinated lignin, steam explosion lignin, ground wood lignin or sulfur lignin; preferably at least one selected from alkali lignin or enzymatic lignin; and/or
The thickening agent is an amide thickening agent, preferably at least one of acrylamide/2-acrylamide-2-methylpropanesulfonic acid copolymer, and the weight average molecular weight of the thickening agent is 500-3000 ten thousand; preferably 1000 to 2000 ten thousand.
4. The lignin-based composite channeling sealing agent according to claim 1, characterized in that:
the stabilizer is selected from at least one of sodium thiosulfate, sodium sulfite, sodium bisulfite, sodium dithionite, isoascorbic acid or thiourea; and/or
The mineralization degree of the prepared water is lower than 200000mg/L.
5. The lignin-based composite channeling sealing agent according to claim 1, wherein the preparation method of the modified cross-linking agent comprises the following steps:
premixing water, phenol, aldehyde, nitrile rubber and organic bentonite, adding an alkali catalyst, and heating for reaction; and after the reaction is finished, adjusting the pH value, and distilling to obtain the modified crosslinking agent.
6. The lignin-based composite channeling sealing agent according to claim 5,
the phenol is selected from at least one of phenol, hydroquinone, resorcinol or catechol; and/or
The aldehyde is selected from at least one of formaldehyde, acetaldehyde or furfural; and/or
The alkali catalyst is soluble alkali, preferably at least one of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate or sodium bicarbonate.
7. The lignin-based composite channeling sealing agent according to claim 5,
the mass ratio of the phenol to the aldehyde to the nitrile rubber is 1: (1.5-4): (0.01-0.05); preferably 1: (1.6-3): (0.02-0.04);
the concentration of the phenol is 1.5-3wt%;
the concentration of the organic bentonite is 0.5-2.5wt%;
the concentration of the alkali catalyst is 0.5-1wt%;
the pH value is adjusted to 7.5-9.5.
8. The lignin-based composite channeling sealing agent according to claim 5,
the heating reaction temperature is 78-88 ℃, and the reaction time is 30-90min;
the distillation mode is vacuum distillation; distilling until the solid content is more than or equal to 40 percent.
9. The preparation method of the lignin-based composite channeling sealing agent according to any one of claims 1 to 8, comprising the steps of:
(1) Adding the thickening agent into prepared water for full dissolution, then adding lignin and a stabilizing agent, and uniformly mixing to obtain a mixed solution;
(2) And (3) dripping a modified cross-linking agent into the mixed solution, uniformly mixing, and then adjusting the pH value to obtain the lignin-based composite channeling sealing agent.
10. The method for preparing lignin-based composite channeling sealing agent according to claim 9,
in the step (2),
adjusting the pH value to 8-11; preferably 9-10.
11. The use of the lignin-based composite channeling sealing agent according to any one of claims 1 to 8 in heavy oil recovery.
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