CN107312517A - A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time - Google Patents
A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time Download PDFInfo
- Publication number
- CN107312517A CN107312517A CN201710471043.1A CN201710471043A CN107312517A CN 107312517 A CN107312517 A CN 107312517A CN 201710471043 A CN201710471043 A CN 201710471043A CN 107312517 A CN107312517 A CN 107312517A
- Authority
- CN
- China
- Prior art keywords
- acid
- preparation
- crosslinking
- organic
- controllable
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002253 acid Substances 0.000 title claims abstract description 115
- 238000004132 cross linking Methods 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000004971 Cross linker Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229920002907 Guar gum Polymers 0.000 claims description 8
- 239000000665 guar gum Substances 0.000 claims description 8
- 229960002154 guar gum Drugs 0.000 claims description 8
- 235000010417 guar gum Nutrition 0.000 claims description 8
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 claims description 7
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 235000011187 glycerol Nutrition 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 4
- -1 carboxy-methyl hydroxy propyl Chemical group 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 229920013818 hydroxypropyl guar gum Polymers 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 3
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- HIPVJRPEJALNIE-UHFFFAOYSA-L [Na+].[K+].OS([O-])=O.OS([O-])=O Chemical compound [Na+].[K+].OS([O-])=O.OS([O-])=O HIPVJRPEJALNIE-UHFFFAOYSA-L 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000003125 aqueous solvent Substances 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 238000005469 granulation Methods 0.000 claims description 2
- 230000003179 granulation Effects 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 claims description 2
- 239000000176 sodium gluconate Substances 0.000 claims description 2
- 235000012207 sodium gluconate Nutrition 0.000 claims description 2
- 229940005574 sodium gluconate Drugs 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 5
- 239000012530 fluid Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 6
- 230000020477 pH reduction Effects 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 238000010276 construction Methods 0.000 description 31
- 239000004576 sand Substances 0.000 description 16
- 238000013461 design Methods 0.000 description 14
- 230000000694 effects Effects 0.000 description 10
- 230000035699 permeability Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 150000001299 aldehydes Chemical class 0.000 description 5
- 238000005457 optimization Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 235000011116 calcium hydroxide Nutrition 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000009671 shengli Substances 0.000 description 2
- 150000005206 1,2-dihydroxybenzenes Chemical class 0.000 description 1
- 241000985905 Candidatus Phytoplasma solani Species 0.000 description 1
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Substances C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/90—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/24—Bacteria or enzyme containing gel breakers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention belongs to acidification of oil field fracturing technique field, the preparation method of the ground composite crosslinking acid of specifically related to a kind of Controllable cross-linking time, the present invention is primarily directed to the existing crosslinking uncontrollable shortcoming of acid fluid system crosslinking time, it is controllable there is provided a kind of crosslinking time, compound acid fluid system of heatproof and preparation method thereof, solve acid fluid system present in conventional acid fracturing underground crosslinked, the uncontrollable shortcoming of crosslinking time, it is of the invention mainly to utilize two kinds of crosslinking agents of different nature and crosslinking conditioner, by adjusting proportioning, control acid fluid system crosslinking time, simultaneously, due to introducing organic resin in system, improve the temperature tolerance of acid fluid system.
Description
Technical field
The present invention relates to the controllable ground composite crosslinking acid of crosslinking time, belong to acidification of oil field fracturing technique field.
Background technology
Conventional ACID FRACTURING TECHNOLOGY has been oil field mature technology, but conventional acid fracturing is present that acid-etched fracture is shorter, flow conductivity is relatively low
Shortcoming, in recent years each research unit carried out retarded acid, turned to acid, foamed acid, the research of the ACID FRACTURING TECHNOLOGY such as underground crosslinked acid
Using, wherein, the multistage ACID FRACTURING TECHNOLOGY of the preferable gel acid of effect is widely used in Shengli Oil Field, but this kind of acid solution
It is uncontrollable to there is crosslinking time in system, occurs that the temperature low cross-linking time is slow, temperature is high and is crosslinked too in the winter time or in hot weather construction
Fast shortcoming, is subject to certain restrictions the application of gel acid ACID FRACTURING TECHNOLOGY.Therefore, with reference to the characteristics of Bin Nanyou areas, to solve
The demand of part Various Seasonal construction, has researched and developed new terrestrial cross-linked acid, by ground cross-linked acid crosslinking time, rheology
Property, the experiment such as temperature tolerance and oil gas field field test, as a result show, ground surface crosslinking acid, realize ground friendship first at home
Connection time controllable characteristic, the construction success of the sour ACID FRACTURING TECHNOLOGY of ground surface crosslinking particularly carried out at oil gas field scene, mark
The formation that a kind of new terrestrial is crosslinked technic acid.
The content of the invention
When the present invention is crosslinked primarily directed to the existing crosslinking uncontrollable shortcoming of acid fluid system crosslinking time there is provided one kind
Between controllable, heatproof compound acid fluid system and preparation method thereof, solve that acid fluid system present in conventional acid fracturing is underground crosslinked, hand over
Connection time uncontrollable shortcoming, the present invention mainly using two kinds of crosslinking agents of different nature and crosslinking conditioner, is matched somebody with somebody by adjustment
Than controlling acid fluid system crosslinking time, simultaneously as introducing organic resin in system, improving the temperature tolerance of acid fluid system.
And be achieved through the following technical solutions：
A kind of preparation method of the controllable ground surface crosslinking acid of crosslinking time is as follows according to mass percent component：Including poly-
Compound viscous acid, combinational organic croslinkers, crosslinking accelerator, are in mass ratio polymer viscous acid：Combinational organic croslinkers：Hand over
Join accelerator=5-8：4-6：3-5, preparation method comprises the following steps：
The preparation of polymer viscous acid：Compound concentration 10-25% hydrochloric acid 1L, adds high molecular polymer, fully dissolving,
4h is stood, guar gum is added, stirred to being fully swelled, polymer thickening acid solution is obtained.
The high molecular polymer be acrylamide, AMPS, SSS, -vinyl-pyrrolidone copolymerization and
Into molecular weight 800-1200 ten thousand.
Itself salt tolerance of the AMPS is preferable, and the SSS hydrophily and salt-resistance are preferable, the N- second
Its copolymerization under certain condition preferably, is obtained high molecular polymer by enyl-pyrrolidine ketone dispersiveness, and the resistance to of its own gently resists
Salt is preferable.
The preparation of the high molecular polymer, is made up of following Material Percentage：Acrylamide 5-30%, AMPS5-
20%, SSS 1-10%, -vinyl-pyrrolidone 0.5-2%, surplus is water.
The preparation method of the high molecular polymer：4 kinds of reaction raw materials are dissolved in the water, the pH value of solution is adjusted
For 8-11, control solution temperature adds oxidation-reducting system initiator potassium peroxydisulfate-Asia under 10-15 DEG C, nitrogen protective condition
Niter cake, triggers 15-20min, and temperature rises to 60-70 DEG C, reacts 3-4h, obtains the gelinite of polymer, dries, granulation,
High molecular polymer is obtained after crushing, 0.05-0.3g initiators are added in every aqueous solution.
The guar gum is hydroxypropyl guar gum or carboxy-methyl hydroxy propyl guar gum.
The high molecular weight water soluble polymer and the mass ratio of guar gum are 7：3.Under such mass ratio, two kinds of polymer
Preferably, and the introducing of guar gum reduces the production cost of polymer viscous acid to solute effect in hydrochloric acid.
The preparation of combinational organic croslinkers：Combinational organic croslinkers are by organic metal titanium crosslinkers and organic borate cross-linker
It is composited.
The preparation method of the organic metal titanium crosslinkers：Organic titanate, alcamine compound are mixed, stirred
Under the conditions of mixing, 60 DEG C are warming up to, keeping temperature is constant, after reaction 40-60min, are continuously heating to 65 DEG C and start distillation, distillation temperature
75-78 DEG C of degree holding is constant, and cut, which reaches, is cooled to less than 60 DEG C after 10-15%, add organic solvent, stir stand-by.
The organic titanate is metatitanic acid tetrem propyl propionate.
The alcamine compound is triethanolamine.
Metatitanic acid tetrem propyl propionate in the reaction raw materials：Triethanolamine：The mass ratio of organic solvent is 1:(2-3):(3-
4)。
The preparation method of the organic borate cross-linker：Water and glycerine are mixed, under stirring condition, 55 are warming up to
DEG C, keeping temperature is constant, after reaction 30min, is continuously heating to 60 DEG C, add after borax and sodium hydroxide, stirring 60min until
All dissolvings, are continuously heating to 65 DEG C, add after stabilizer and part, stirring 2h, stop reaction, obtain organic borate cross-linker.
The stabilizer is sodium thiosulfate.
The part is one or both of lactic acid or sodium gluconate.
The mass ratio of the aqueous solvent and glycerine is 3:1.
The reaction raw materials reclaimed water：Glycerine：Sodium hydroxide：Borax：Stabilizer：The mass ratio of part is (40-58)：
(15-20):(2-8)：(10-20)：(2-10)：(2-5).
The mass ratio of the organic metal titanium crosslinkers and organic borate cross-linker is 7:3, under the conditions of the ratio, cross-linking effect
Most preferably.
The preparation of crosslinking accelerator：Control below 30 DEG C of temperature, after aldehyde material and aldehydes matter are mixed completely, slowly
40 DEG C are warming up to, highly basic is added, 45 DEG C are to slowly warm up to, weak base is added, is to slowly warm up at 55 DEG C, 55-60 DEG C of keeping temperature
3h is reacted, less than 30 DEG C is cooled the temperature to, obtains crosslinking accelerator product.
The aldehyde material is the formalin solution of 35-40% concentration.
The aldehydes matter is phenol.
The highly basic is one kind in sodium hydroxide or potassium hydroxide.
The weak base is one kind in ammoniacal liquor or calcium hydroxide.
Aldehyde in the reaction raw materials：Phenol：Highly basic：The mass ratio of weak base is 1:(2-4)：(0.01-0.05)：(0.01-
0.05)。
The preparation method of the controllable ground surface crosslinking acid of crosslinking time：Added into the polymer viscous acid prepared organic
Multiple crosslinking agent, after stirring, adds crosslinking accelerator, continues to stir, and finally obtains the controllable ground of crosslinking time and hands over
Connection acid.
During the addition combinational organic croslinkers, mixing speed is 100-200r/min, and mixing time is 3-5min.
During the addition crosslinking accelerator, mixing speed is 100-200r/min, and mixing time is 1-3min.
This product has the following advantages that compared with existing product：
1st, the features such as product has good heatproof, salt resistance, resistant to shearing, thorough strong, the broken glue of prop-carrying capacity.
(1) in 120 DEG C of heatproof resistant to shearing rheological characteristic experiments, after shearing 120min, viscosity B coefficent is more stable, is maintained at
More than 60-75mPa.s；In 140 DEG C of heatproof resistant to shearing rheological characteristic experiments, after shearing 120min, viscosity B coefficent is more stable, protects
Hold in more than 60-70mPa.s, show good heatproof resistant to shearing intensity.
(2) in the raw material of synthesising macromolecule copolymer, the preferable thing of the salt-resistances such as AMPS and SSS is added
Matter so that the polymer being synthesized has good salt resistance effect.
(3) 48h, when crosslinked fluid sand ratio is 30-40%, the ceramsite propping agent for still having more than 95% suspends, and does not occur bright
Aobvious sand fallout, sedimentation phenomenon, it is shown that good solid-carrying performance.
(4) cross-linked acid can complete rapid break in 3.5h, meet the rapid break and the need for the row of returning of job site requirement
Ask.
2nd, the characteristics of product has crosslinking time, cross-link intensity is controllable.
(1) ground surface crosslinking acid group is actual according to ground construction requirement and well depth, design delay crosslinking time, in laboratory experiment,
Crosslinking time is controllable in 20-300s.
(2) ground surface crosslinking acid can be according to target reservoir temperature adjustment respective strengths, and the viscosity after crosslinking is can be controlled in
150-260mPa.s。
3rd, the product selects new polymer viscous acid and combinational organic croslinkers, not only forms new cross-linked acid production
Product, and it is truly realized the controllability of crosslinking time.
Brief description of the drawings
Fig. 1：Polymer viscous acid outward appearance；
Fig. 2：Composite crosslinking acid frozen glue outward appearance；
Fig. 3：The fresh acid of cross-linked acid；
Fig. 4：The residual acid of cross-linked acid；
Fig. 2-Fig. 4 is the photo for hanging phenomenon after the controllable acid fluid system crosslinking of crosslinking time of the present invention；
Fig. 5：Shore 105-17 well acid fracturing construction curves；
Fig. 6：3 sand groups and 4 sand group anti-fittings calculate fracture pattern；
Fig. 7：1 sand group and 2 sand group construction crack form anti-fitting results；
Fig. 8：Production curve after the acid fracturing construction curve of embodiment 2 and pressure；
Fig. 9：Production curve after the acid fracturing construction curve of embodiment 2 and pressure；
Figure 10：The shore 644X36 well construction curves of embodiment 3；
Figure 11：Comparative example shore 644X43 well construction curves.
Embodiment
Embodiment 1
The present embodiment is the Bin105-17Jing of 105 pieces of Shengli Oil Field shore, and its major oil reservoir is s_4 formation reservoir, with psephitic sand
Based on rock, permeability is 23~148.3 × 10-3μm2, mean permeability 62 × 10-3μm2, it is hypotonic-hypotonic for low hole-mesopore, spy
Reservoir, porosity is distributed between 14.6~21.7%, average pore 17.5%；Main Reservoirs lithology is with shale cryptocrystal ash
Based on rock, average limestone content 50% or so is more complicated with low hole-mesopore, special hypotonic-hypotonic physical property characteristic and lithology
Limestone feature, 2700~2900m of reservoir buried depth, acid fracturing target zone bottom hole temperature (BHT) is up to 120 DEG C.
It is prepared as follows the ground composite crosslinking acid of Controllable cross-linking time：
(1) polymer viscous acid is prepared：15% hydrochloric acid 1L is prepared with running water to add in reaction vessel, while stirring slowly
5.0g high molecular polymers are added, and continue stirring and are allowed to abundant dissolving, places 2 hours, 2.0g carboxylics is added under agitation
Methylhydroxypropyl guar gum, continues to stir up to uniform, stand-by.The typical preparation method of high molecular polymer：Acrylamide
Above-mentioned raw materials are well mixed by 20%, AMPS15%, SSS 5%, -vinyl-pyrrolidone 1%, water 59%,
It is 8.5 to adjust pH value, and control solution temperature adds oxidation-reducting system initiator persulfuric acid under 15 DEG C, nitrogen protective condition
Potassium-sodium hydrogensulfite, triggers 20min, and temperature rises to 70 DEG C, reacts 3h, obtains the gelinite of polymer, dries, and granulates, and crushes
After obtain high molecular polymer.
(2) combinational organic croslinkers are prepared：Weigh 15.1g metatitanic acid tetrems propyl propionate to add in three-necked flask, in heating
Triethanolamine 34.7g is added, under the conditions of 60 DEG C, is reacted 40 minutes, 65 DEG C is warming up to and starts distillation, vapo(u)rizing temperature is maintained at
75-78 DEG C, when cut amount reaches 6.4mL, it is cooled to after less than 60 DEG C and adds methanol, stir stand-by.Organic boron is added to hand over
Join agent, stir, it is stand-by.
(3) crosslinking accelerator is prepared：In with condenser pipe, thermometer, the three-necked flask of agitator, 79.2g good fortune is added
You are Malin, adds 22.5g phenol below 30 DEG C of temperature of control, is to slowly warm up to 40 DEG C, adds 0.05g sodium hydroxides, be warming up to
45 DEG C, 1 hour heating-up time.0.05g calcium hydroxides are added, 55 DEG C, 1 hour heating-up time are warming up to.It is anti-in the insulation of 55-60 degree
Answer 3 hours, be cooled to 30 DEG C with bottom discharge.
(4) 5.0g combinational organic croslinkers are added in the polymer viscous acid 7.0g prepared, are stirred 4 minutes, then are added
Enter 3.0g crosslinking conditioners, stir 2 minutes, obtain ground surface crosslinking acid.
Multistage acid fracturing construction has been carried out to Bin105-17Jing on December 26th, 2015.This construction is applied according to optimization design
Engineering sequence is carried out, and has carried out safety, smoothly construction operation to the sand group of shore 105-17 wells 3 and 4 sand groups first, then pitching point
Every to 1 sand group and the multistage acid fracturing construction of 2 sand groups progress, whole reservoir reconstruction process is performed by optimization design substantially.This construction
Fracturing unit is arranged to march into the arena since morning, operation team connection fracture manifold and instrument monitoring circuit, 2 pm, all prepared just
Thread, turn on pump pressure testing.High pressure pipe joint highest pressure testing 75MPa, steady pressure 3min, do not occur to pierce leakage situation, are set then according to optimization
The sand group of meter construction pump ordered pair 3 and 4 sand groups carry out acid fracturing construction, terminate rear pitching and set to carry out acid fracturing to 1 sand group and 2 sand groups and apply
Work.This construction well head adds up feed liquor 352m3, wherein 3 sand groups and 4 sand group feed liquor 187m3, 1 sand group and 2 sand group feed liquor 165m3,
With designing total liquid measure 380m3, 3 sand groups and 4 sand group 205m3, 1 sand group and 2 sand group 175m3Basically identical, operational discharge capacity is also by design
4m3/ min is implemented, and has reached Optimizing construction, the purpose of safe and smooth construction.
Using three-dimensional acid fracturing design software is intended, according to construction data, calculating, practice of construction fracture pattern knot are simulated
Fruit such as Fig. 6.Contrast design and anti-fitting result of calculation are visible (table 1.1), the fracture parameters and optimization design after practice of construction
Fracture parameters relatively, have reached the requirement of design.Simulative display construction after acid-etched fracture have preferable fracture length and
Zero dimension flow conductivity, illustrates that pit shaft is linked up in crack and the ability on stratum is preferable, fluid has higher permeability in crack.
1.1 acid fracturing anti-fittings calculate acid-etched fracture parameter
Fig. 7 is the anti-fitting fracture pattern result of 1 sand group and 2 sand groups.Contrast design parameter is visible (table 1.2), actually applies
Fracture parameters after work are sufficiently close to optimal design parameter, the acid-etched fracture that construction is formed have certain fracture length and compared with
High zero dimension flow conductivity, with the higher ability for linking up pit shaft and stratum filtration.
The sand group of table 1.2 1 and 2 sand group anti-fittings calculate acid-etched fracture parameter
Open flow returns row after acid fracturing
Bin105-17Jing constructs when 26 days 17 December in 2015 to be terminated, and is reacted 2 hours by design closing well, table 1.3 is recorded
The row of returning situation after well acid, as a result shows, well head pressure declines fast, and decrease speed returns alignment profit close to 2MPa/h.
Open flow is recorded after the shore 105-17 acid fracturings of table 1.3
The broken glue that proving the ground composite crosslinking acid has had returns row's ability.
The shore 105-17 well effect tables of table 1.4
Embodiment 2：
It is prepared by ground surface crosslinking acid：
(1) polymer viscous acid is prepared：15% hydrochloric acid 1L is prepared with distilled water, three mouthfuls with stirring and thermometer are added
In flask, 4.0g high molecular polymers are slowly added to while stirring, and continue stirring to be allowed to abundant dissolving, place 2 hours, stirring
1.7g carboxy-methyl hydroxy propyl guar gums are added under the conditions of mixing, continue to stir up to uniform, it is stand-by.
(2) combinational organic croslinkers are prepared：10.7g metatitanic acid tetrems propyl propionate is weighed to add with condenser pipe adopter, temperature
In degree meter, the three-necked flask of agitator, diethanol amine 24.5g is added in heating, under the conditions of 60 DEG C, reacts 40 minutes, rises
Temperature starts to distill to 65 DEG C, and vapo(u)rizing temperature is maintained at 75-78 DEG C, when cut amount reaches 6.4mL, is cooled to addition after less than 60 DEG C
Methanol, stirs stand-by.
(3) crosslinking accelerator is prepared：In with condenser pipe, thermometer, the three-necked flask of agitator, 79.2g good fortune is added
You are Malin, adds 22.5g phenol below 30 DEG C of temperature of control, is to slowly warm up to 40 DEG C, adds 0.05g sodium hydroxides, be warming up to
45 DEG C, 1 hour heating-up time.0.05g calcium hydroxides are added, 55 DEG C, 1 hour heating-up time are warming up to.It is anti-in the insulation of 55-60 degree
Answer 3 hours, be cooled to 30 DEG C with bottom discharge.
(4) 6.0g combinational organic croslinkers are added in the polymer viscous acid 8.0g prepared, are stirred 3 minutes, then are added
Enter 4.0g crosslinking conditioners, stirring 2min obtains ground surface crosslinking acid.
The cross-linked acid prepared with this kind of method has carried out acid fracturing construction in September, 2015 in stake Gu 10-13 wells.Working procedure
Carried out by optimization design, squeeze into ground composite crosslinking acid 200m3, liquid nitrogen 10m3.Whole work progress is more smooth.Well head ruptures
Pressure 48.55Pa, converts bottom hole fracturing pressure (BHFP) 66.26MPa, fracture pressure gradient 0.0191MPa/m；Well head instantaneous characteristics
11.97MPa, achieves good effect.Production curve is shown in Fig. 8 and Fig. 9 after specific acid fracturing construction curve and pressure.
Embodiment 3
It is prepared by ground surface crosslinking acid：
It is prepared by ground surface crosslinking acid：
(1) polymer viscous acid is prepared：20% hydrochloric acid 1000mL is prepared with distilled water, is added with stirring and thermometer
In three-necked flask, 5.0g high molecular polymers are slowly added to while stirring, and continue stirring to be allowed to abundant dissolving, place 2 hours,
It is stand-by.
(2) organo-metallic crosslinker is prepared：6.2g metatitanic acid tetrems propyl propionate, which is added, carries condenser pipe, thermometer, agitator
Three-necked flask in, stirring it is fully dissolved, be slowly added to 14.0g triethanolamines, at 90 DEG C, react 4 hours, be down to normal temperature
Discharging.
(3) crosslinking accelerator is prepared：In with condenser pipe, thermometer, the three-necked flask of agitator, 79.2g good fortune is added
You are Malin, adds 19.1g catechols below 30 DEG C of temperature of control, is to slowly warm up to 40 DEG C, add 0.05g sodium hydroxides, rises
Temperature is to 45 DEG C, 1 hour heating-up time.0.05g calcium hydroxides are added, 55 DEG C, 1 hour heating-up time are warming up to.In 55-60 DEG C of guarantor
Temperature reaction 3 hours, is cooled to 30 DEG C with bottom discharge.
(4) 5.0g organo-metallic crosslinkers are added in the polymer viscous acid 5.0g prepared, are stirred 5 minutes, then are added
Enter 4.0g crosslinking conditioners, stirring obtains ground surface crosslinking acid for 1 minute.
Ground composite crosslinking acid prepared by Application Example 3 has carried out acid fracturing in Bin644X36Jing in November, 2016 and applied
Work, works well.
Top surface construction is overall relatively easy on the sand four of 644 blocks of shore, and lithology is siltstone and coarse powder sandstone, median grain diameter
0.06mm, rock particles is thinner, buried depth of top surface 2510m~2770m.1 sand group reservoir porosity is 17% on the sand four of 644 blocks of shore,
Permeability is 76 × 10-3μm2, 2 sand group reservoir porosities are 16.1% on the sand four of 644 blocks of shore, and permeability is 46 × 10-3μm2, shore
3 sand group reservoir porosities are 14.8% on 644 blocks of sand four, and permeability is 28.6 × 10-3μm2, 4 sand groups storage on the sand four of 644 blocks of shore
Layer porosity is 15.2%, and permeability is 20.5 × 10-3μm2, belong to middle low permeability reservoir.The upper original formation pressures of Sha Si
26MPa, pressure coefficient 0.96, formation temperature is in 94-118 DEG C, 3.4 DEG C/100m of geothermal gradient.
Shore 644X36 wells 2016.11.1 has carried out pressing crack construction.Well target zone span 52.8m, span is larger, using machine
Tool separate stratum fracfturing mode.Stratum energy is low, whole with fluid injection nitrogen in fracturing process, improves stratum energy.By production engineering specifications
First layer is co-extruded into prepad fluid 75m3, ground composite crosslinking acid 83m3, replace 17m3, liquid nitrogen 6m3, design sand 14m3, it is actual to add
Sand 8.4m3, most high sand ratio 11.5%, fracture pressure 51.5MPa, termination of pumping pressure 23MPa.The second layer is co-extruded into prepad fluid 54m3, ground
Face composite crosslinking acid 80.3m3, replace 15.5m3, liquid nitrogen 6m3, design sand 12m3, actual plus sand 7.1m3, most high sand ratio
12.5%, fracture pressure 50.7MPa, termination of pumping pressure 20.8MPa, construction are smooth.
Effect see the table below 1.5.
Comparative example：
Using common cross-linked acid in the Bin644X43Jing of the block of identical shore 644, Contrast on effect has been carried out.
Shore 644X43 wells 2016.10.31 has carried out pressing crack construction, and prepad fluid 10m is co-extruded into by production engineering specifications3, it is general
Logical gel acid 118.4m3, replace 16.1m3, add up fracturing fluid 144.5m3, design sand 10m3, actual plus sand 7.3m3, most STOL
Than 23%, operational discharge capacity is controlled in 1.5-5m3/ min, fracture pressure 51.6MPa, termination of pumping pressure 23.1MPa.Constructing, all are suitable
Profit.
Effect see the table below 1.5.
644 pieces of 1.5 shore of table, two mouthfuls of well effect tables
Claims (10)
1. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time, it is characterised in that including polymer viscous acid,
Combinational organic croslinkers, crosslinking accelerator, are in mass ratio polymer viscous acid：Combinational organic croslinkers：Crosslinking accelerator=
5-8：4-6：3-5, preparation method comprises the following steps：
(1) preparation of polymer viscous acid：Compound concentration 10-25% hydrochloric acid 1L, adds high molecular polymer, fully dissolving,
4h is stood, guar gum is added, stirred to being fully swelled, polymer thickening acid solution is obtained；
The preparation of the high molecular polymer, is made up of following Material Percentage：Acrylamide 5-30%, AMPS5-20%,
SSS 1-10%, -vinyl-pyrrolidone 0.5-2%, surplus is water；The high molecular polymer molecular weight is
800-1200 ten thousand；
(2) preparation of combinational organic croslinkers：Combinational organic croslinkers are by organic metal titanium crosslinkers and organic borate cross-linker
It is composited；
(3) preparation of crosslinking accelerator：Control below 30 DEG C of temperature, after aldehyde material and aldehydes matter are mixed completely, slowly
40 DEG C are warming up to, highly basic is added, 45 DEG C are to slowly warm up to, weak base is added, is to slowly warm up at 55 DEG C, 55-60 DEG C of keeping temperature
3h is reacted, less than 30 DEG C is cooled the temperature to, obtains crosslinking accelerator；
(4) preparation method of the controllable ground surface crosslinking acid of crosslinking time：Added into the polymer viscous acid prepared organic
Multiple crosslinking agent, after stirring, adds crosslinking accelerator, continues to stir, and finally obtains the controllable ground of crosslinking time and hands over
Connection acid.
2. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In the preparation method of high molecular polymer described in step (1)：Above-mentioned 4 kinds of reaction raw materials are dissolved in the water, adjustment solution
PH value is 8-11, and control solution temperature adds oxidation-reducting system initiator persulfuric acid under 10-15 DEG C, nitrogen protective condition
Potassium-sodium hydrogensulfite, triggers 15-20min, and temperature rises to 60-70 DEG C, reacts 3-4h, obtains the gelinite of polymer, dries,
Granulation, high molecular polymer is obtained after crushing, and 0.05-0.3g initiators are added in every aqueous solution.
3. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In the preparation method of organic metal titanium crosslinkers described in step (2)：Organic titanate, alcamine compound are blended in one
Rise, under stirring condition, be warming up to 60 DEG C, keeping temperature is constant, after reaction 40-60min, be continuously heating to 65 DEG C and start distillation,
75-78 DEG C of vapo(u)rizing temperature holding is constant, and cut, which reaches, is cooled to less than 60 DEG C after 10-15%, add organic solvent, stir
It is stand-by.
4. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In the preparation method of organic borate cross-linker described in step (2)：Water and glycerine are mixed, under stirring condition, heating
To 55 DEG C, keeping temperature is constant, after reaction 30min, is continuously heating to 60 DEG C, adds after borax and sodium hydroxide, stirring 60min
Until all dissolvings, are continuously heating to 65 DEG C, add after stabilizer and part, stirring 2h, stop reaction, obtain organic boron crosslinking
Agent.
5. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In guar gum described in step (1) is hydroxypropyl guar gum or carboxy-methyl hydroxy propyl guar gum；High molecular polymer described in step (1)
Mass ratio with guar gum is 7：3.
6. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In organic titanate described in step (2) is metatitanic acid tetrem propyl propionate；
Alcamine compound described in step (2) is triethanolamine；
Metatitanic acid tetrem propyl propionate in reaction raw materials described in step (2)：Triethanolamine：The mass ratio of organic solvent is 1:(2-3):
(3-4)。
7. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In stabilizer described in step (2) is sodium thiosulfate；
Part described in step (2) is one or both of lactic acid or sodium gluconate；
The mass ratio of aqueous solvent and glycerine described in step (2) is 3:1.
8. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In reaction raw materials reclaimed water described in step (2)：Glycerine：Sodium hydroxide：Borax：Stabilizer：The mass ratio of part is (40-
58)：(15-20):(2-8)：(10-20)：(2-10)：(2-5)；
The mass ratio of organic metal titanium crosslinkers and organic borate cross-linker described in step (2) is 7:3.
9. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In aldehyde material described in step (3) is the formalin solution of 35-40% concentration；
Aldehydes matter described in step (3) is phenol；
Highly basic described in step (3) is one kind in sodium hydroxide or potassium hydroxide；
Weak base described in step (3) is one kind in ammoniacal liquor or calcium hydroxide；
Aldehyde in reaction raw materials described in step (3)：Phenol：Highly basic：The mass ratio of weak base is 1:(2-4)：(0.01-0.05)：
(0.01-0.05)。
10. a kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time according to claim 1, its feature exists
In when adding combinational organic croslinkers described in step (4), mixing speed is 100-200r/min, and mixing time is 3-5min；
When adding crosslinking accelerator described in step (4), mixing speed is 100-200r/min, and mixing time is 1-3min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710471043.1A CN107312517A (en) | 2017-06-20 | 2017-06-20 | A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710471043.1A CN107312517A (en) | 2017-06-20 | 2017-06-20 | A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107312517A true CN107312517A (en) | 2017-11-03 |
Family
ID=60181997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710471043.1A Pending CN107312517A (en) | 2017-06-20 | 2017-06-20 | A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107312517A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276982A (en) * | 2018-03-22 | 2018-07-13 | 昆山京昆油田化学科技开发公司 | A kind of organic titanium cross-linking agent and its preparation method and application |
| CN108822827A (en) * | 2018-07-21 | 2018-11-16 | 东营市宝泽能源科技有限公司 | A kind of superhigh temperature cross-linked acid |
| CN111057532A (en) * | 2018-10-17 | 2020-04-24 | 中国石油化工股份有限公司 | Fracturing crosslinking agent and guar gum fracturing fluid |
| CN111349427A (en) * | 2018-12-20 | 2020-06-30 | 中石化石油工程技术服务有限公司 | Temperature-controlled fracturing fluid |
| CN116854857A (en) * | 2023-07-10 | 2023-10-10 | 山东诺尔生物科技有限公司 | Composition for preparing water-absorbent resin fiber, water-absorbent resin fiber and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005099654A1 (en) * | 2004-04-19 | 2005-10-27 | Wsp Chemicals & Technology, Llc | Water soluble polymer complexes with surfactants |
| CN103805158A (en) * | 2012-11-09 | 2014-05-21 | 中国石油化工股份有限公司 | Cross-linked acid acidizing fracturing fluid, preparation method and application thereof |
| CN104073237A (en) * | 2014-06-03 | 2014-10-01 | 中国石油天然气股份有限公司 | High-temperature-resistant ground crosslinked acid solution and preparation method thereof |
| CN104403658A (en) * | 2014-12-08 | 2015-03-11 | 中国石油大学(华东) | High-temperature-resistant crosslinking acid liquor system as well as preparation method thereof |
| CN105542068A (en) * | 2014-10-24 | 2016-05-04 | 中国石油化工股份有限公司 | Hydrophobically-associating polyacrylamide fracturing fluid thickener, preparation method and applications thereof |
| CN105646777A (en) * | 2015-12-29 | 2016-06-08 | 四川光亚聚合物化工有限公司 | Hydrophobic associated polymer and preparation method thereof |
| CN106008803A (en) * | 2016-05-26 | 2016-10-12 | 中国石油集团渤海钻探工程有限公司 | High temperature resistant cross-linked acid thickening agent and preparation method thereof |
| CN106433588A (en) * | 2016-09-05 | 2017-02-22 | 中国石油天然气集团公司 | Compound crosslinking agent, preparation method of compound crosslinking agent and preparation method of profile control agent |
-
2017
- 2017-06-20 CN CN201710471043.1A patent/CN107312517A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005099654A1 (en) * | 2004-04-19 | 2005-10-27 | Wsp Chemicals & Technology, Llc | Water soluble polymer complexes with surfactants |
| CN103805158A (en) * | 2012-11-09 | 2014-05-21 | 中国石油化工股份有限公司 | Cross-linked acid acidizing fracturing fluid, preparation method and application thereof |
| CN104073237A (en) * | 2014-06-03 | 2014-10-01 | 中国石油天然气股份有限公司 | High-temperature-resistant ground crosslinked acid solution and preparation method thereof |
| CN105542068A (en) * | 2014-10-24 | 2016-05-04 | 中国石油化工股份有限公司 | Hydrophobically-associating polyacrylamide fracturing fluid thickener, preparation method and applications thereof |
| CN104403658A (en) * | 2014-12-08 | 2015-03-11 | 中国石油大学(华东) | High-temperature-resistant crosslinking acid liquor system as well as preparation method thereof |
| CN105646777A (en) * | 2015-12-29 | 2016-06-08 | 四川光亚聚合物化工有限公司 | Hydrophobic associated polymer and preparation method thereof |
| CN106008803A (en) * | 2016-05-26 | 2016-10-12 | 中国石油集团渤海钻探工程有限公司 | High temperature resistant cross-linked acid thickening agent and preparation method thereof |
| CN106433588A (en) * | 2016-09-05 | 2017-02-22 | 中国石油天然气集团公司 | Compound crosslinking agent, preparation method of compound crosslinking agent and preparation method of profile control agent |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276982A (en) * | 2018-03-22 | 2018-07-13 | 昆山京昆油田化学科技开发公司 | A kind of organic titanium cross-linking agent and its preparation method and application |
| CN108822827A (en) * | 2018-07-21 | 2018-11-16 | 东营市宝泽能源科技有限公司 | A kind of superhigh temperature cross-linked acid |
| CN111057532A (en) * | 2018-10-17 | 2020-04-24 | 中国石油化工股份有限公司 | Fracturing crosslinking agent and guar gum fracturing fluid |
| CN111349427A (en) * | 2018-12-20 | 2020-06-30 | 中石化石油工程技术服务有限公司 | Temperature-controlled fracturing fluid |
| CN111349427B (en) * | 2018-12-20 | 2022-08-09 | 中石化石油工程技术服务有限公司 | Temperature-controlled fracturing fluid |
| CN116854857A (en) * | 2023-07-10 | 2023-10-10 | 山东诺尔生物科技有限公司 | Composition for preparing water-absorbent resin fiber, water-absorbent resin fiber and preparation method thereof |
| CN116854857B (en) * | 2023-07-10 | 2024-07-23 | 山东诺尔生物科技有限公司 | Composition for preparing water-absorbent resin fiber, water-absorbent resin fiber and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107312517A (en) | A kind of preparation method of the ground composite crosslinking acid of Controllable cross-linking time | |
| US20170015889A1 (en) | Degradable materials for oil and gas field operations and their synthesis method | |
| CN110257031A (en) | Oil field microparticle hydrogel profile control water shutoff agent and preparation method thereof | |
| CN107629774A (en) | A kind of temporarily stifled diversion agent and preparation method thereof | |
| CN102562021B (en) | Quick gel breaking process for intermediate and low temperate oil gas well fracturing fluid | |
| CN111793485B (en) | Water shutoff agent and preparation method and application thereof | |
| NO178471B (en) | Method for preparing wellbore in fluid communication with an underground hydrocarbon bearing formation as well as pressure cementing method applied to a lined wellbore | |
| NO178472B (en) | Method for preparing wellbore by sealing an unlined wall in a wellbore and method for drilling and clarifying a radius and a horizontal wellbore | |
| CN106433601A (en) | Crosslinking agent for sea water-based fracturing fluid as well as preparation method and application of crosslinking agent | |
| CN113201855B (en) | Full-degradable high-strength temporary knot plug | |
| CN109439310A (en) | high-temperature guanidine gum fracturing fluid and preparation method thereof | |
| CN110079286A (en) | Delayed crosslinking gel composition for plugging and preparation method thereof | |
| CN106382113A (en) | Temporary plugging steering acidification method applicable to sandstone reservoir | |
| CN112341997A (en) | High-temperature-resistant gel plugging agent for oil-based drilling fluid and preparation method and application thereof | |
| CN108955404A (en) | A kind of perforating oil gas well pressure break super powder charge and preparation method | |
| CN103342879B (en) | Degradable temporary plugging ball | |
| CN105131931A (en) | 200 DEG C high temperature resistance fracturing construction jelly preparation method | |
| CN113528098A (en) | Ductile particle plugging system for fracture lost drilling and plugging and preparation method thereof | |
| CN112094629A (en) | Plugging agent suitable for fractured oil reservoir | |
| CN112175599B (en) | Alkali-resistant coating sand and preparation method and application thereof | |
| CN112876612A (en) | Temperature-sensitive low-fluid-loss underground cross-linking agent for plugging cracks and application thereof | |
| CN110790959A (en) | Water-soluble phenolic resin crosslinking agent low-temperature rapid gelling and crosslinking promoting agent and preparation method and application thereof | |
| CN103849363B (en) | A kind of thermal recovery vapour alters improvement gel-like double-liquid seal blocking agent and method for blocking thereof | |
| CN105567200B (en) | A kind of preparation method of biogel profile control agent | |
| CN106497100B (en) | The emulsification method of bitumen regenerant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171103 |