CN106589257A - Preparation method of lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent - Google Patents
Preparation method of lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent Download PDFInfo
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- CN106589257A CN106589257A CN201611126938.3A CN201611126938A CN106589257A CN 106589257 A CN106589257 A CN 106589257A CN 201611126938 A CN201611126938 A CN 201611126938A CN 106589257 A CN106589257 A CN 106589257A
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- lignin
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- plugging agent
- water
- polymer
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- 229920005610 lignin Polymers 0.000 title claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229920000642 polymer Polymers 0.000 title claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005189 flocculation Methods 0.000 title claims abstract description 12
- 230000016615 flocculation Effects 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000002091 cationic group Chemical group 0.000 claims abstract description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 10
- 238000007334 copolymerization reaction Methods 0.000 claims description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 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
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims 2
- 239000000047 product Substances 0.000 claims 2
- 150000002500 ions Chemical class 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 8
- 238000005406 washing Methods 0.000 abstract description 6
- 238000002347 injection Methods 0.000 abstract description 5
- 239000007924 injection Substances 0.000 abstract description 5
- 230000001376 precipitating effect Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000011435 rock Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 229920006318 anionic polymer Polymers 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000005465 channeling Effects 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000005611 electricity Effects 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 150000001768 cations Chemical class 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- -1 acrylyl Chemical group 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical group [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 239000002349 well water Substances 0.000 description 1
- 235000020681 well water Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/514—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides a lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent and a preparation method thereof. The preparation process comprises the following steps: firstly, purifying lignin; secondly, adding 500 to 800 parts of de-ionized water, 50 to 200 parts of an acrylamide monomer and 10 to 20 parts of a cationic monomer into a reaction container; introducing nitrogen gas and stirring; raising the temperature to be 50 DEG C; adding 10 to 20 parts of purified lignin and adding 0.05 to 0.1 part of an initiator; keeping the heat and reacting for 6h to 8h; precipitating and separating an obtained product with acetone; after washing with diethyl ether, drying to obtain a finished product. The polymer flocculation type profile modifying/water plugging agent provided by the invention can directly react with an anionic polymer; after reaction, generated flocs can be firmly adsorbed on surfaces of rocks with negative electricity, which are washed by water for a long period; the plugging strength is high and the washing resisting performance is good. The profile modifying/water plugging agent is used for carrying out deep profile modification after polymer flooding by sufficiently utilizing underground residual polymers after the polymer flooding; after the profile modifying/water plugging agent is injected into the ground, polymers from an injection end or remained in a stratum can be continuously captured and the permeability of a high-permeability layer is greatly reduced, so that the production cost is reduced and fluid channeling of sequent water flooding after the polymer flooding is inhibited.
Description
Technical field
The present invention relates to a kind of preparation method of the polymer flocculation type profile-controlling and plugging agent of lignin graft copolymerization.
Background technology
Since tertiary oil recovery polymer flooding industrialization promotion, the effect of preferable oil increasing precipitation, postpolymer flood have been achieved
There is substantial amounts of polymer residual liquid in underground, after recovery water drive, due to irrational mobility, when the reason such as the anisotropism on stratum is made
The fingering phenomenon of Cheng Shui, substantially reduces the swept volume of injection water, makes the extraction well water logging quickly of postpolymer flood, High water cut,
High universal containing poly- situation, the inefficient cycle of polymer causes oil well productivity to decline to a great extent, and suppresses the channelling of sequent water flooding after poly- drive,
Improving water drive swept volume becomes problem demanding prompt solution, and residual polyalcohol reutilization technology and Novel technique of in-depth profile control are poly- at present
The emphasis direction of yield-increasing technology research after compound drive.
Polymer flocculants profile control technique is mainly polymerized with oil reservoir by injecting the polymer flocculants of sodium great soil group at present
Thing generation flocculation of meeting is deposited in high permeability zone, reaches the purpose of closure high permeability zone, but such granular profile control agent belongs to inorganic
Profile control agent, it is larger to formation damage, it is water insoluble, and granule deformation behavior is poor, is not easily accessible oil reservoir deep, not reaching makes liquid stream exist
The purpose that oil reservoir deep turns to.Therefore the polymer flocculation type profile-controlling and plugging agent of offer a kind of " enter and must go " and " stifled to live ",
Profile control is carried out with very real meaning using the substantial amounts of polymer residual liquid in underground after poly- drive.
The content of the invention
The technical problem to be solved in the present invention is that the polymer flocculation type profile control for providing a kind of lignin graft copolymerization is blocked up
The preparation method of water preparation.
A kind of preparation method of graft copolymerization polymer flocculation type profile-controlling and plugging agent includes：
First by lignin and 20% sodium hydroxide solution hybrid reaction, PH is adjusted to 1～2 with hydrochloric acid, filter out precipitation
Thing, water washing and precipitating thing to PH obtain purification lignin after being dried in the range of 6～7.
(500～800) part deionized water, (50～200) part acrylamide monomer, (10～20) are added in reaction vessel
Part cationic monomer, logical nitrogen are simultaneously stirred, and are warming up to 50 DEG C, add (10～20) part purification lignin, are added (0.05～0.1)
The initiator of part, 6～8h of insulation reaction, products therefrom are separated with acetone precipitation, be dried, obtain finished product after ether cleaning.
Preferably, the initiator is Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, ammonium sulfite, sodium sulfite, thio
One or more in sodium sulfate, hydrogen peroxide, triethanolamine；
Preferably, described cationic monomer has following structure：
Wherein, R1=(- H), (- CH3), R2=it is (- CH3)、(-C2H5), R3=(- CH3)、(-C2H5)、(-C2H4OH)
Preferably, described lignin is alkali lignin.
The present invention is had the advantage that and beneficial effect compared with prior art：
The polymer flocculation type profile-controlling and plugging agent that the present invention is provided, directly can be reacted with anionic polymer, be not required to
To compound with other materials, it is to avoid the chromatographic fractionation effect of multicomponent profile control system；One of blocking agent primary raw material lignin is honest and clean
Valency is easy to get, and production cost is low compared with common cation polymer；Generate floccule body firmly to adsorb for a long time by water punching after reaction
The electronegative rock surface of brush, plugging strength are high, and flushing resistance is good.The profile-controlling and plugging agent is present in after making full use of poly- drive
Underground residual polymer carries out deep profile controlling after poly- drive, can persistently trap and retain in injection end or stratum behind injection underground
Polymer, the permeability of high permeability zone is greatly lowered, so as to reduce production cost, after suppressing poly- drive, sequent water flooding alters
Stream.
Specific embodiment
With reference to specific embodiment, and the present invention is described in further detail according to data.It should be understood that these embodiments
It is of the invention solely for the purpose of illustration, rather than the scope of the present invention is limited by any way.
Embodiment 1：
A kind of preparation of graft copolymerization cation profile-controlling and plugging agent, it is composed of the following components：
Wherein, cationic monomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, and structural formula is as follows：
Preparation technology：
First by lignin and 20% sodium hydroxide solution hybrid reaction, PH is adjusted to 1～2 with hydrochloric acid, filter out precipitation
Thing, water washing and precipitating thing to PH obtain purification lignin after being dried in the range of 6～7.
615 parts of deionized waters, 105 parts of acrylamide monomers, 10 parts of cationic monomers are added in reaction vessel, leads to nitrogen
And stir, 50 DEG C are warming up to, 70 parts of purification lignins are added, 0.03 part of potassium peroxydisulfate, 0.03 part of sodium sulfite is added, insulation is anti-
Answer 8h, products therefrom to be separated with acetone precipitation, be dried after ether cleaning, obtain finished product.
Embodiment 2：
A kind of preparation of graft copolymerization cation profile-controlling and plugging agent, it is composed of the following components：
Wherein, cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, and structural formula is as follows：
Preparation technology：
First by lignin and 20% sodium hydroxide solution hybrid reaction, PH is adjusted to 1～2 with hydrochloric acid, filter out precipitation
Thing, water washing and precipitating thing to PH obtain purification lignin after being dried in the range of 6～7.
620 parts of deionized waters, 120 parts of acrylamide monomers, 15 parts of cationic monomers are added in reaction vessel, leads to nitrogen
And stir, 50 DEG C are warming up to, 45 parts of purification lignins are added, 0.03 part of potassium peroxydisulfate, 0.03 part of sodium thiosulfate, insulation is added
Reaction 8h, products therefrom are separated with acetone precipitation, be dried, obtain finished product after ether cleaning.
Embodiment 3：
A kind of preparation of graft copolymerization cation profile-controlling and plugging agent, it is composed of the following components：
Wherein, cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac, and structural formula is as follows：
Preparation technology：
First by lignin and 20% sodium hydroxide solution hybrid reaction, PH is adjusted to 1～2 with hydrochloric acid, filter out precipitation
Thing, water washing and precipitating thing to PH obtain purification lignin after being dried in the range of 6～7.
575 parts of deionized waters, 120 parts of acrylamide monomers, 10 parts of cationic monomers are added in reaction vessel, leads to nitrogen
And stir, 50 DEG C are warming up to, 90 parts of purification lignins are added, 0.04 part of potassium peroxydisulfate, 0.04 part of sodium thiosulfate, insulation is added
Reaction 6h, products therefrom are separated with acetone precipitation, be dried, obtain finished product after ether cleaning.
The shut-off capacity of profile-controlling and plugging agent of the present invention is evaluated using artificial homogenizing rock core, and experimentation is：By three pieces
Long 30cm, sectional area 4.5*4.5cm2Simulation core, be respectively labeled as 1#、2#、3#、4#, which is surveyed after water drive to pressure stability and is blocked up
Front permeability Kw0, 0.5PV common anion polyacrylamide solutions (molecular weight 19,000,000, concentration 1800mg/L) are then injected into,
The profile control agent of variable concentrations is prepared, and the liquid of 0.2PV mesh is injected from injection end or production end, is subsequently injected into 0.1PV water and is pushed up
Replace, at 45 DEG C, be incubated 72h, water drive is steady to pressure again, survey stifled rear permeability K of rock corew1, and according to formulaCalculate sealing ratiod E.
Test result indicate that, plugging agent of the present invention have very strong sealing characteristics, relatively low concentration can just reach compared with
Good plugging effect, ensure that effectively closure high permeability zone, and after a large amount of waterflood flushes, sealing ratiod fall is less, resistance to erosion
Better performances.
In sum, presently preferred embodiments of the present invention is these are only, is not intended to limit protection scope of the present invention.
Therefore, all any modification, equivalent substitution and improvements made within the spirit and principles in the present invention etc., should be included in this
Within bright protection domain.
Claims (5)
1. the preparation method of the polymer flocculation type profile-controlling and plugging agent of a kind of lignin graft copolymerization, it is characterised in that：Its molecule
General structure is：
Wherein, R1=(- H), (- CH3), R2=it is (- CH3)、(-C2H5), R3=(- CH3)、(-C2H5)、(-C2H4OH),
Liginin represents lignin molecule chain.
2. the preparation side of the polymer flocculation type profile-controlling and plugging agent of a kind of lignin graft copolymerization according to claim 1
Method, it is characterised in that：Processing preparation process is as follows：
First by lignin and 20% sodium hydroxide solution hybrid reaction, PH is adjusted to 1～2 with hydrochloric acid, filter out precipitate, water
Precipitate is washed to PH in the range of 6～7, after being dried, obtain purification lignin.
(500～800) part deionized water, (50～200) part acrylamide monomer, (10～20) part sun are added in reaction vessel
Ion monomer, logical nitrogen are simultaneously stirred, and are warming up to 50 DEG C, are added (10～20) part purification lignin, add (0.05～0.1) part
Initiator, 6～8h of insulation reaction, products therefrom are separated with acetone precipitation, be dried, obtain finished product after ether cleaning.
3. preparation method according to claim 2, it is characterised in that：The initiator is Ammonium persulfate., potassium peroxydisulfate, mistake
One or more in sodium sulfate, ammonium sulfite, sodium sulfite, sodium thiosulfate, hydrogen peroxide, triethanolamine.
4. preparation method according to claim 2, it is characterised in that：The cationic monomer for being used has following structure：
Wherein, R1=(- H), (- CH3), R2=it is (- CH3)、(-C2H5), R3=(- CH3)、(-C2H5)、(-C2H4OH)。
5. preparation method according to claim 2, it is characterised in that：Described lignin is alkali lignin.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018161164A1 (en) * | 2017-03-09 | 2018-09-13 | Fpinnovations | Process for producing cationic lignin copolymer under aqueous acid conditions |
| CN108795399A (en) * | 2018-08-17 | 2018-11-13 | 佛山朝鸿新材料科技有限公司 | A kind of frozen glue packer material and preparation method thereof |
| CN110002563A (en) * | 2019-04-17 | 2019-07-12 | 山东大学 | A kind of preparation method of high molecular weight paper mill sludge base organic cation flocculating agent |
| CN110628399A (en) * | 2018-06-22 | 2019-12-31 | 中国石油天然气股份有限公司 | Plugging agent for plugging cracks and plugging method thereof |
| CN112175592A (en) * | 2019-07-02 | 2021-01-05 | 中石化南京化工研究院有限公司 | Dendritic cationic polyacrylamide coating agent for water-based drilling fluid and preparation method thereof |
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