CN107722143A - A kind of preparation method and fracturing fluid system of alcohol ether modified guar - Google Patents
A kind of preparation method and fracturing fluid system of alcohol ether modified guar Download PDFInfo
- Publication number
- CN107722143A CN107722143A CN201711063864.8A CN201711063864A CN107722143A CN 107722143 A CN107722143 A CN 107722143A CN 201711063864 A CN201711063864 A CN 201711063864A CN 107722143 A CN107722143 A CN 107722143A
- Authority
- CN
- China
- Prior art keywords
- alcohol ether
- fracturing fluid
- present
- guar
- preparation
- Prior art date
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 254
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000012530 fluid Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 244000007835 Cyamopsis tetragonoloba Species 0.000 title claims abstract 7
- 239000000243 solution Substances 0.000 claims abstract description 62
- 229920002907 Guar gum Polymers 0.000 claims abstract description 51
- 239000000665 guar gum Substances 0.000 claims abstract description 51
- 229960002154 guar gum Drugs 0.000 claims abstract description 51
- 235000010417 guar gum Nutrition 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 238000006277 sulfonation reaction Methods 0.000 claims abstract description 40
- 239000003513 alkali Substances 0.000 claims abstract description 29
- 239000002585 base Substances 0.000 claims abstract description 26
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
- YYROPELSRYBVMQ-UHFFFAOYSA-N 4-toluenesulfonyl chloride Chemical compound CC1=CC=C(S(Cl)(=O)=O)C=C1 YYROPELSRYBVMQ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012670 alkaline solution Substances 0.000 claims abstract description 19
- 239000003292 glue Substances 0.000 claims description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 238000005956 quaternization reaction Methods 0.000 claims description 18
- 239000012190 activator Substances 0.000 claims description 17
- 239000003002 pH adjusting agent Substances 0.000 claims description 17
- 239000004927 clay Substances 0.000 claims description 16
- 230000000844 anti-bacterial effect Effects 0.000 claims description 15
- 239000003899 bactericide agent Substances 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- 229910052708 sodium Inorganic materials 0.000 claims description 15
- 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 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000003381 stabilizer Substances 0.000 claims description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 8
- 150000001638 boron Chemical class 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
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical group N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 12
- 239000004576 sand Substances 0.000 abstract description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 8
- 230000036571 hydration Effects 0.000 abstract description 5
- 238000006703 hydration reaction Methods 0.000 abstract description 5
- 125000004430 oxygen atom Chemical group O* 0.000 abstract description 4
- 230000008961 swelling Effects 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 112
- 244000303965 Cyamopsis psoralioides Species 0.000 description 49
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- 239000007788 liquid Substances 0.000 description 21
- 235000011121 sodium hydroxide Nutrition 0.000 description 17
- -1 toluene Sulphonic acid ester Chemical class 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 238000000605 extraction Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000003921 oil Substances 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 8
- 238000005660 chlorination reaction Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- 230000004913 activation Effects 0.000 description 5
- 239000005457 ice water Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229920000570 polyether Polymers 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 4
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 4
- 102000008186 Collagen Human genes 0.000 description 4
- 108010035532 Collagen Proteins 0.000 description 4
- 241000219112 Cucumis Species 0.000 description 4
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 4
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 229910021538 borax Inorganic materials 0.000 description 4
- 229920001436 collagen Polymers 0.000 description 4
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004328 sodium tetraborate Substances 0.000 description 4
- 235000010339 sodium tetraborate Nutrition 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 229960001716 benzalkonium Drugs 0.000 description 3
- CYDRXTMLKJDRQH-UHFFFAOYSA-N benzododecinium Chemical compound CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 CYDRXTMLKJDRQH-UHFFFAOYSA-N 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- 229920006317 cationic polymer Polymers 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N methylene chloride Substances ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 3
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000000811 xylitol Substances 0.000 description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 3
- 229960002675 xylitol Drugs 0.000 description 3
- 235000010447 xylitol Nutrition 0.000 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 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 206010010214 Compression fracture Diseases 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000176 sodium gluconate Substances 0.000 description 2
- 235000012207 sodium gluconate Nutrition 0.000 description 2
- 229940005574 sodium gluconate Drugs 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BBDNZMUIQBRBJH-UHFFFAOYSA-N sulfurochloridic acid;toluene Chemical compound OS(Cl)(=O)=O.CC1=CC=CC=C1 BBDNZMUIQBRBJH-UHFFFAOYSA-N 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- SLPVJDQRGMDQLQ-UHFFFAOYSA-N 2-hydroxyhex-2-enoic acid Chemical class CCCC=C(O)C(O)=O SLPVJDQRGMDQLQ-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000521257 Hydrops Species 0.000 description 1
- 241000406668 Loxodonta cyclotis Species 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- WRLRISOTNFYPMU-UHFFFAOYSA-N [S].CC1=CC=CC=C1 Chemical compound [S].CC1=CC=CC=C1 WRLRISOTNFYPMU-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008953 bacterial degradation Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012458 free base Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229960001031 glucose Drugs 0.000 description 1
- 235000001727 glucose Nutrition 0.000 description 1
- 229920000591 gum Polymers 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002631 hypothermal effect Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000009671 shengli Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/0096—Guar, guar gum, guar flour, guaran, i.e. (beta-1,4) linked D-mannose units in the main chain branched with D-galactose units in (alpha-1,6), e.g. from Cyamopsis Tetragonolobus; Derivatives thereof
-
- 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
- C09K8/605—Compositions for stimulating production by acting on the underground formation containing biocides
-
- 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
- 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
- C09K2208/26—Gel breakers other than bacteria or enzymes
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Emergency Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Cosmetics (AREA)
Abstract
The invention provides a kind of preparation method of alcohol ether modified guar and a kind of fracturing fluid, the present invention realizes the basification to alcohol ether by strong base solution, and then it is easy to the reaction between alcohol ether and paratoluensulfonyl chloride, and by the way that paratoluensulfonyl chloride organic solution is added drop-wise in the alcohol ether alkali；Sulfonation alcohol ether is added dropwise in the alkaline solution of raw material guar gum again, realize grafting, obtain alcohol ether modified guar, so that contain more oxygen atoms and hydroxyl in the structure of guar gum, 3 D stereo rock-steady structure, and then fully hydration swelling under cryogenic are formed with crosslinking agent, discharges viscosity, added in fracturing fluid with low concentration, ensure the sand carrying effect of fracturing fluid.The result of embodiment shows, alcohol ether modified guar is prepared using the present invention, is added to 0.1~0.3% concentration in fracturing fluid, still can ensure that excellent sand carrying effect, reaches 24h without sedimentation.
Description
Technical field
The present invention relates to oil exploitation auxiliary agent technical field, more particularly to a kind of preparation method of alcohol ether modified guar and
Fracturing fluid.
Background technology
Along with North America shale gas revolution, stimulation technology is leading the great of global unconventionaloil pool exploration and development
Change, have become the three big crucial engineering technology arranged side by side with physical prospecting, drilling well.Reservoir reconstruction object complex, there is conventional storage
Layer and unconventional reservoir, and reservoir properties have Thief zone, hyposmosis and Oil in Super-low Permeability, or even receive darcy level compact reservoir.In order to
Preferably implement reservoir reconstruction, adaptation method, wherein hydraulic fracturing must be used for the reservoir reconstruction object of different physical property
A kind of important well stimulation as transformation low permeability pay is more and more extensive in each field use in China.
Waterpower oil field compression fracture natural plant gum mainly has guar gum, xanthans and starch, and wherein xanthans, starch etc. is glued by it
Spending relatively low property influences, and is used in hydraulic fracturing field less.At present, guar gum is widely used for being applied to Shengli Oil
Field, Daqing oil field, extend domestic each elephant such as oil field, also have with country in the area such as North America, Southeast Asia, the Central Asia and Russia
Huge market.
The need of the exploitation to fine and close oil, shale oil gas, guar gum and its derived product are continued to increase recently as China
The amount of asking increases year by year., more need to be 2% but at the scene in order to increase sand carrying effect in use, the concentration of guar gum is higher
Left and right, and higher guar gum concentration can cause the injury to stratum flow conductivity, influence production of hydrocarbons efficiency.
The content of the invention
It is an object of the invention to provide a kind of preparation method and fracturing fluid of alcohol ether modified guar, the present invention is prepared into
To alcohol ether modified guar still ensure that with relatively low concentration the sand carrying effect of fracturing fluid.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of preparation method of alcohol ether modified guar, comprise the following steps：
(1) alcohol ether organic solution is mixed with strong base solution, carries out quaternization, obtain alcohol ether alkali；
(2) after paratoluensulfonyl chloride organic solution being added drop-wise to the alcohol ether alkali that the step (1) obtains, sulfonation is continued
Reaction, obtains sulfonation alcohol ether；The speed of the dropwise addition is 20~32mL/h；
(3) after the organic solution of the obtained sulfonation alcohol ether being added dropwise into the alkaline solution of guar gum, continue to be grafted
Reaction, obtains alcohol ether modified guar；The speed of the dropwise addition is 8~10mL/h.
Preferably, the temperature of quaternization is 0~5 DEG C in the step (1), and the time of quaternization is 10~15min.
Preferably, the temperature of sulfonating reaction is 0~5 DEG C in the step (2)；The time of sulfonating reaction is 2.5~3h.
Preferably, the temperature of graft reaction is 63~66 DEG C in the step (3)；The time of graft reaction is 10~12h.
Present invention also offers a kind of fracturing fluid, include the component of following weight/mass percentage composition：Described in above-mentioned technical proposal
The alcohol ether modified guar 0.1~0.35% that preparation method is prepared, clay stabilizer 0.1~0.3%, bactericide 0.1~
0.2%, Waterproof lock agent 0.25~0.3%, crosslinking agent 0.15~0.4%, gel breaker 0.04~0.06%, the broken glue activator of low temperature
0.01~0.03%, surplus is water and alkaline pH adjuster；
The dosage of the alkaline pH adjuster is defined by that can obtain the fracturing fluid that pH value is 8.5~12.
Preferably, the clay stabilizer is the polymeric quartenary ammonium that potassium chloride, ammonium chloride or relative molecular weight are less than 5000
Salt.
Preferably, the crosslinking agent is organic boron complexes.
Preferably, the Waterproof lock agent is OPEO or NPE.
Preferably, the gel breaker is the one or more in ammonium sulfate, potassium peroxydisulfate and ammonium persulfate.
Preferably, for activate the low temperature of the gel breaker break glue activator be glucose, 2,3,5,6- tetrahydroxy -2- oneself
One or more in olefin(e) acid -4- lactones sodium and citric acid.
The invention provides a kind of preparation method of alcohol ether modified guar, comprise the following steps：By alcohol ether organic solution
Mixed with strong base solution, carry out quaternization, obtain alcohol ether alkali；Obtained by paratoluensulfonyl chloride organic solution is added drop-wise to again
After alcohol ether alkali, continue sulfonating reaction, obtain sulfonation alcohol ether；It is 20~32mL/h to control the speed being added dropwise；Then, by gained
To sulfonation alcohol ether organic solution be added dropwise to the alkaline solution of raw material guar gum after, continue graft reaction, obtain alcohol ether and change
Property guar gum；The speed of the dropwise addition is 8~10mL/h.
The present invention realizes the basification to alcohol ether by strong base solution, and then is easy between alcohol ether and paratoluensulfonyl chloride
Reaction, and by the way that paratoluensulfonyl chloride organic solution is added drop-wise into the temperature effectively controlled in the alcohol ether alkali in mixed process
Degree, then sulfonation alcohol ether is added dropwise in the alkaline solution of raw material guar gum, the grafting between alcohol ether and guar gum is realized, obtains alcohol ether
Modified guar, realize and alcohol ether is accessed in guar gum so that contain more oxygen atoms and hydroxyl in the structure of guar gum, can
3 D stereo rock-steady structure is more fully formed with crosslinking agent, this structure can make its fully hydration swelling under cryogenic,
Viscosity is discharged, is added in fracturing fluid with low concentration, you can ensure the performance of fracturing fluid, it is ensured that sand carrying effect.Implement
The result of example shows, alcohol ether modified guar is prepared using the present invention, is added to 0.1~0.3% guar concentrations
In fracturing fluid, excellent sand carrying effect is still can ensure that, reaches 24h without sedimentation.
Brief description of the drawings
Fig. 1 is the temperature and shearing sustainability testing result curve map for the corresponding frozen glue of fracturing fluid that comparative example 1 of the present invention obtains；
Fig. 2 is the temperature and shearing sustainability testing result curve map for the corresponding frozen glue of fracturing fluid that the embodiment of the present invention 3 obtains.
Embodiment
The invention provides a kind of preparation method of alcohol ether modified guar, comprise the following steps：
(1) alcohol ether organic solution is mixed with strong base solution, carries out quaternization, obtain alcohol ether alkali；
(2) after paratoluensulfonyl chloride organic solution being added drop-wise to the alcohol ether alkali that the step (1) obtains, sulfonation is continued
Reaction, obtains sulfonation alcohol ether；The speed of the dropwise addition is 20~32mL/h；
(3) after the organic solution of the obtained sulfonation alcohol ether being added dropwise into the alkaline solution of raw material guar gum, continue
Graft reaction, obtain alcohol ether modified guar；The speed of the dropwise addition is 8~10mL/h.
The present invention mixes alcohol ether organic solution with strong base solution, carries out quaternization, obtains alcohol ether alkali.In the present invention
In, the alcohol ether is preferably diglycol or triethylene-glycol；Organic solvent is preferably in the alcohol ether organic solution
Tetrahydrofuran or dioxane.In the present invention, the molar concentration of the alcohol ether organic solution is preferably (1~4) mol/L, is entered
One step is preferably (2~3) mol/L.In the present invention, the strong base solution is preferably sodium hydroxide solution and/or potassium hydroxide
Solution；Solvent is preferably water in the strong base solution；The concentration of the strong base solution is preferably (4~8) mol/L, further excellent
Elect (5~7) mol/L, more preferably 6mol/L as.In the present invention, the mol ratio of the alcohol ether and highly basic be preferably (0.1~
0.2)：(0.2~0.4), more preferably (0.1~0.15)：(0.25~0.3).
In the present invention, the temperature of the quaternization is preferably 0~5 DEG C, more preferably 3~4 DEG C；The alkalization
The time of reaction is preferably 10~15min, more preferably 12~13min.Specific reality of the present invention to the quaternization
The mode of applying does not have particular/special requirement, using embodiment well-known to those skilled in the art；In an embodiment of the present invention,
The quaternization is carried out preferably under the conditions of ice-water bath.In the present invention, the quaternization is preferably entered under agitation
OK.The present invention realizes the alkalization to alcohol ether during the quaternization, by highly basic, obtains alcohol ether alkali；When the highly basic
When solution is sodium hydroxide solution, by the quaternization, alcohol ether sodium is generated；When the strong base solution is potassium hydroxide,
By the quaternization, alcohol ether potassium is generated.
After quaternization, after paratoluensulfonyl chloride organic solution is added drop-wise to the alcohol ether alkali by the present invention, continue sulphur
Change reaction, obtain sulfonation alcohol ether.In the present invention, organic solvent is preferably tetrahydrochysene furan in the paratoluensulfonyl chloride organic solution
Mutter or dioxane.In the present invention, the molar concentration of the paratoluensulfonyl chloride organic solution is preferably (1.25~5) mol/
L, more preferably (2.5~3) mol/L.In the present invention, counted on the basis of the dosage of alcohol ether during quaternization, institute
The mol ratio for stating paratoluensulfonyl chloride and alcohol ether is preferably (0.1~0.2)：(0.1~0.2).
The present invention does not have particular/special requirement to the source of the paratoluensulfonyl chloride, and use is well-known to those skilled in the art
Commercial goods.
In the present invention, the speed that paratoluensulfonyl chloride organic solution is added dropwise is (20~32) mL/h, is preferably (25
~30) mL/h.In the present invention, the sulfonating reaction between paratoluensulfonyl chloride and alcohol ether alkali occurs during the dropwise addition, sternly
Lattice control drop rate, avoid disposable add from mixing, produce accessory substance.In the present invention, the temperature during the dropwise addition
Preferably 0~5 DEG C, more preferably 1~4 DEG C, more preferably 2~3 DEG C.Embodiment of the present invention to the dropwise addition
There is no particular/special requirement, using dropwise addition mode well-known to those skilled in the art；In an embodiment of the present invention, the drop
Process is added preferably to be carried out under water bath condition；When the heat for reacting discharged causes the no longer described dropping temperature scope of system temperature
It is interior, the regulation and control to temperature are specifically realized by the way of extraneous temperature adjustment.
The present invention occurs between toluene sulfochloride and alcohol ether alkali during paratoluensulfonyl chloride is added drop-wise to alcohol ether alkali
Sulfonating reaction.
In the present invention, the time of the dropwise addition is preferably 2~2.5h.The paratoluensulfonyl chloride is completed to alcohol ether alkali
After dropwise addition, the present invention is preferably further continued for 2.5~3h of carry out reaction.In the present invention, the time of the sulfonating reaction is preferably
2.5~3h.In the present invention, the time of the sulfonating reaction is added drop-wise to after alcohol ether alkali completely by paratoluensulfonyl chloride start in terms of.
In the present invention, the temperature of the sulfonating reaction is preferably 0~5 DEG C, more preferably 1~4 DEG C, more preferably 2~3 DEG C.
During the sulfonating reaction, the present invention carries out sulfonation by toluene sulfochloride to the alcohol ether alkali, obtains alcohol ether to toluene
Sulphonic acid ester, i.e. sulfonation alcohol ether.When the alcohol ether is diglycol, obtained sulfonation alcohol ether is diglycol single pair
Tosylate；When the alcohol ether is triethylene-glycol, obtained sulfonation alcohol ether is triethylene-glycol single pair toluene sulphur
Acid esters.
After the sulfonating reaction, the obtained reaction material liquid is preferably extracted and dried successively by the present invention, is obtained
Sulfonation alcohol ether.In the present invention, the extraction more preferably uses CH successively2Cl2The reaction material liquid is extracted with water
Take.In the present invention, the extraction is preferably after the reaction material liquid is mixed with frozen water, using CH2Cl2It is extracted twice, separates
Obtain just extraction oily liquids；The obtained first extraction oily liquids is washed twice using water, isolated deep extraction oily liquids.
The present invention does not have particular/special requirement to the embodiment of the extraction, using extraction mode well-known to those skilled in the art
.
After obtaining deep extraction oily liquids, the obtained deep extraction oily liquids is dried the present invention, obtains sulfonation alcohol
Ether.In the present invention, the drying preferably includes to use anhydrous MgSO4Mistake after primary is dried is carried out to the deep extraction oily liquids
Filter, obtains filtrate；The filtrate is evaporated, the organic solvent in filtrate is removed, obtains sulfonation alcohol ether.The present invention is to described
The embodiment that primary is dry, filters and is evaporated does not have particular/special requirement, using implementation well-known to those skilled in the art
Mode is can realize the removal of moisture in sulfonation alcohol ether.
After obtaining sulfonation alcohol ether, the organic solution of the obtained sulfonation alcohol ether is added dropwise to raw material guar gum by the present invention
After organic solution, continue graft reaction, obtain alcohol ether modified guar.
In the present invention, the preparation method of the alkaline solution of the raw material guar gum preferably includes：By having for raw material guar gum
Machine solution mixes with highly basic, is alkalized, and obtains the alkaline solution of raw material guar gum.
In the present invention, the alkalization guar gum is preferably sodium hydroxide or potassium hydroxide with highly basic.In the present invention, institute
It is preferably (10~20) to state the mass ratio of raw material guar gum and highly basic in the organic solution of raw material guar gum：(0.1~0.2), enters
One step is preferably 15：(0.1~0.2).In the present invention, organic solvent is preferably four in the organic solution of the raw material guar gum
Hydrogen furans or dioxane.In the present invention, guar gum or HPG based on the raw material guar gum is preferred；This hair
The bright source to the basic guar gum and HPG does not have a particular/special requirement, and use is well-known to those skilled in the art
Commercial goods；In an embodiment of the present invention, the basic guar gum is specially the commercial goods of Guar collagen powder.At this
In invention, the quality of raw material guar gum and the volume ratio of organic solvent are preferably (10 in the organic solution of the raw material guar gum
~20) g：(100~200) mL, more preferably (15~18) g：(150~180) mL.
In the present invention, the temperature that the guar gum is alkalized is preferably 0~5 DEG C, more preferably 3~4 DEG C；Institute
The time for stating alkalization is preferably 0.5~1h.After the present invention mixes the organic solution of raw material guar gum with highly basic, in the temperature
Under time conditions, the hydroxyl reaction of highly basic and guar gum is realized, the structure of similar sodium alkoxide is generated, obtains the alkali of raw material guar gum
Compound；The guar gum of alkalization is more convenient for carrying out graft reaction with sulfonation alcohol ether.
In the present invention, the dosage of the alkaline solution of the organic solution of the sulfonation alcohol ether and raw material guar gum is with sulfonation alcohol ether
And counted in the alkaline solution preparation process of raw material guar gum on the basis of the dosage of raw material guar gum, the material of the sulfonation alcohol ether
The mass ratio of amount and raw material guar gum is preferably 0.04mol：(10~20) g, more preferably 0.04mol：(12~18) g,
More preferably 0.04mol：16g.
In the present invention, organic solvent is preferably tetrahydrofuran or dioxane in the organic solution of the sulfonation alcohol ether.
In the present invention, the concentration of the organic solution of the sulfonation alcohol ether is preferably 0.2mol/L~0.25mol/L.
The present invention by the organic solution of the sulfonation alcohol ether be added dropwise to speed in the alkaline solution of raw material guar gum for (8~
10) mL/h, more preferably (8.5~9) mL/h.The present invention is added dropwise to raw material Guar using by the organic solution of sulfonation alcohol ether
Mode in the alkaline solution of glue, strictly controls drop rate, this dropwise addition mode ensure that sulfonation alcohol ether more fully with Guar
Glue completes graft reaction, and side reaction product is considerably less.In the present invention, the temperature of the dropwise addition is preferably 0~5 DEG C, is entered
One step is preferably 3~4 DEG C.
The present invention does not have particular/special requirement to the embodiment of the dropwise addition, and use is well-known to those skilled in the art
Solution dropwise addition mode；In an embodiment of the present invention, the dropwise addition is specifically completed using constant pressure funnel.
During the organic solution of sulfonation alcohol ether is added dropwise to the alkaline solution of raw material guar gum by the present invention, that is, send out sulfonation alcohol
Graft reaction between the alkali compound of ether and raw material guar gum.In the present invention, the temperature of the dropwise addition process be preferably 60~
66 DEG C, more preferably 64~65 DEG C.
In the present invention, the time of the dropwise addition is preferably 2~2.5h.The organic solution of the sulfonation alcohol ether is completed to original
After the dropwise addition for expecting the alkaline solution of guar gum, the present invention preferably continues to 10~12h of carry out reaction.In the present invention, the grafting
The time of reaction is preferably 10~12h.In the present invention, the time of the graft reaction is complete with the organic solution of sulfonation alcohol ether
Start to count after being added drop-wise to the alkaline solution of raw material guar gum.In the present invention, the temperature of the graft reaction is preferably 60~66 DEG C,
More preferably 64~65 DEG C.In the process of grafting, with the guar gum of alkalization William occurs for the alcohol ether of sulfonation
Gloomy ether synthetic reaction, p-methyl benzenesulfonic acid ester group make alcohol ether complete the grafting with guar gum as leaving group.
After the graft reaction, resulting grafting feed liquid is preferably filtered and washed successively by the present invention, obtains alcohol
Ether modified guar.The present invention does not have particular/special requirement to the mode of the filtering, can obtain filter cake.The present invention preferably adopts
The filter cake is washed three times with absolute ethyl alcohol, obtains alcohol ether modified guar；Specific reality of the present invention to the washing
The mode of applying does not have particular/special requirement, using well-known to those skilled in the art.
Alcohol ether modified guar provided by the invention, because the access of alcohol ether so that containing more in the structure of guar gum
Oxygen atom and hydroxyl, 3 D stereo rock-steady structure more fully can be formed with crosslinking agent, this structure can make it in cryogenic conditions
Lower fully hydration swelling, is discharged viscosity, is added in fracturing fluid with low concentration, you can ensure the performance of fracturing fluid, really
Protect sand carrying effect.
Present invention also offers a kind of fracturing fluid, include the component of following weight/mass percentage composition：Described in above-mentioned technical proposal
The alcohol ether modified guar 0.1~0.35% that preparation method is prepared, clay stabilizer 0.1~0.3%, bactericide 0.1~
0.2%, Waterproof lock agent 0.25~0.3%, crosslinking agent 0.15~0.4%, gel breaker 0.04~0.06%, the broken glue activator of low temperature
0.01~0.03%, surplus is water and alkaline pH adjuster；The dosage of the alkaline pH adjuster using can obtain pH value as
8.5~12 fracturing fluid is defined.
In the present invention, the fracturing fluid includes 0.1~0.35% alcohol ether modified guar, preferably 0.11~
0.25%, more preferably 0.15~0.2%.In the present invention, the alcohol ether modified guar is preceding solution institute
The alcohol ether modified guar that preparation method is prepared is stated, will not be repeated here.
In the present invention, the fracturing fluid includes 0.1~0.3% clay stabilizer, preferably 0.15~0.25%, enters
One step is preferably 0.2%.In the present invention, the clay stabilizer is preferably that potassium chloride, ammonium chloride or relative molecular weight are less than
5000 Polymeric quaternary ammonium salts.In the present invention, the relative molecular weight of the Polymeric quaternary ammonium salts is preferably less than 5000, enters one
Step is preferably less than 4500, more preferably 2000~4000；The Polymeric quaternary ammonium salts are preferably the alkyl of Hydrin-eight
Dimethyl tertiary amine quaternary ammonium salt, Hydrin-Dodecyl Dimethyl Amine quaternary ammonium salt or Hydrin-dodecyl
Dimethyl tertiary amine quaternary ammonium salt；The Polymeric quaternary ammonium salts play the effect of cationic polymer, are effectively reduced the suction of layer clay
Water expansion rate.In the present invention, the clay stabilizer can be effectively reduced a layer clay expansion rate of water absorption, and then prevent clay
Excessively gas channel is reduced in expansion causes oil and gas production to decline.
In the present invention, the fracturing fluid includes 0.1~0.2% bactericide.In the present invention, the bactericide is preferred
Chlorination benzalkonium or relative molecular weight are less than 5000 Polymeric quaternary ammonium salts；The relative molecular weight of the Polymeric quaternary ammonium salts is excellent
Elect as less than 5000, more preferably less than 4500, more preferably 2000~4000；The Polymeric quaternary ammonium salts are preferably poly-
The alkyl quaternary ammonium salts of amide amine-chlorination eight, daiamid-chlorination dodecyl quaternary ammonium salt or polyamide amine chlorination dodecyl season
Ammonium salt.In the present invention, the bactericide provides preferably in the form of the bactericide aqueous solution；The present invention is water-soluble to the bactericide
The concentration of liquid does not have particular/special requirement, any concentration ratio.In the present invention, the bactericide can be killed effectively carefully
Bacterium, bacterial degradation modified guar is prevented, and then fully keep the viscosity of modified guar.
In the present invention, the fracturing fluid includes 0.25~0.3% Waterproof lock agent, more preferably 0.26~
0.28%.In the present invention, the Waterproof lock agent is preferably OPEO or NPE；It is described pungent
The polyether units of base phenol polyethenoxy ether and NPE preferably independently for more than 8, more preferably 10~
50, more preferably 15~30.In the present invention, the Waterproof lock agent effectively can prevent or reduce water-blocking effect, and then prevent
Working fluid forms emulsion with crude oil, is effectively reduced water and immerses injury caused by oil reservoir.
In the present invention, the fracturing fluid includes 0.15~0.4% crosslinking agent, preferably 0.2~0.25%.In this hair
In bright, the crosslinking agent is preferably the ligand compound of organic boron complexes, more preferably borate and hydroxy-containing compounds
Thing；The hydroxy-containing compounds are preferably xylitol, glucose or sodium gluconate；The borate be preferably sodium tetraborate or
It is hydrated sodium tetraborate.
In the present invention, the preparation method of organic boron complexes preferably includes：By the borate and hydroxyl
Compound is coordinated under conditions of alkali lye, obtains organic boron complexes.In the present invention, the alkali lye is preferably potassium hydroxide
Solution or sodium hydroxide solution；The mass concentration of the alkali lye is preferably 15~25%, and more preferably 20%.In the present invention
In, the mol ratio of alkali is preferably 1 in the borate, hydroxy-containing compounds and alkali lye:2.In the present invention, the crosslinking agent energy
Enough and base fluid acts on, and realizes the frozen glue of fracturing fluid, is easy to be used to take sand pressure break.
In the present invention, the dosage of the alkaline pH adjuster is defined by that can obtain the fracturing fluid that pH value is 8.5~12,
The pH value of the fracturing fluid is 8.5~12, preferably 9.0~9.5, more preferably 9.5~10.2.In the present invention, institute
The quality for stating alkaline pH adjuster is preferably the 0.3% of fracturing fluid.In the present invention, the alkaline pH adjuster is preferably
Industrial sodium carbonate solid powder or sodium hydroxide solution.In the present invention, when the alkaline pH adjuster is that sodium hydroxide is molten
During liquid, the mass concentration of the sodium hydroxide solution is preferably below 3%.
In the present invention, the fracturing fluid includes 0.04~0.06% gel breaker, preferably includes 0.05%.In the present invention
In, gel breaker preferred sodium peroxydisulfate, potassium peroxydisulfate or the ammonium persulfate.
In the present invention, the fracturing fluid includes 0.01~0.03% low temperature and breaks glue activator, and preferably 0.02%.
In the present invention, the low temperature breaks glue activator and is preferred for activating the gel breaker；The low temperature for being used to activate gel breaker is broken
Glue activator is preferably the one or more in glucose, 2,3,5,6- tetrahydroxys -2- hexenoic acids -4- lactones sodium and citric acid.
In the present invention, when the gel breaker is sodium peroxydisulfate, the low-temp activation gel breaker is preferably glucose or 2, and 3,5,6- tetra-
Hydroxyl -2- hexenoic acids -4- lactones sodium or the composition of glucose and citric acid；It is described low when the gel breaker is potassium peroxydisulfate
The broken glue activator of temperature is preferably 2,3,5,6- tetrahydroxys -2- hexenoic acids -4- lactones sodium or citric acid or glucose and 2,3,5,6-
Composition or glucose, the 2,3,5,6- tetrahydroxys -2- hexenoic acids -4- lactones sodium and lemon of tetrahydroxy -2- hexenoic acid -4- lactone sodium
The composition of lemon acid；When the gel breaker is potassium peroxydisulfate, it is preferably glucose, citric acid or 2 that the low temperature, which breaks glue activator,
3,5,6- tetrahydroxy -2- hexenoic acid -4- lactone sodium.When the present invention breaks glue activator using a variety of low temperature, the present invention is to combination
The dosage that Different hypothermia breaks glue activator in thing does not have particular/special requirement, is mixed with arbitrary proportion.
In the present invention, the gel breaker can effectively cut off the strand of modified guar, form it into small molecular sugar
Class, make frozen glue chemical conversion watery, be easy to the row of returning, reduce level of residue；And the broken glue activator of the low temperature can be at low temperature to breaking glue
Line activating is entered in agent, is able to play the effect of gel breaker.
In the present invention, alcohol ether modified guar in fracturing fluid, clay stabilizer, bactericide, Waterproof lock agent 0.25~
0.3%th, crosslinking agent, alkaline pH adjuster, gel breaker and low temperature break the weight/mass percentage composition of glue activator each component preferably with
Fracturing fluid in the form of frozen glue in the presence of the weight/mass percentage compositions of respective components count.
Melon provided by the invention splits liquid and uses introducing of the alcohol ether modified guar by alcohol ether in modified guar, causes to tie
More oxygen atoms and hydroxyl are provided with structure, fully form 3 D stereo rock-steady structure with crosslinking agent, and then can be in low temperature bar
Fully hydration swelling under part, discharges viscosity, effectively reduces the Applicable temperature of fracturing fluid, widen applicable temperature range, while
The concentration of guar gum in fracturing fluid is not influenceed to reduce on the premise of sand carrying effect；And with reference to described low temperature break glue activator and
Gel breaker, gel breaker is activated under broken glue activator dosage at a lower temperature, relatively low, gel breaker is decomposed release oxygen free
Base so that broken glue is more thoroughly and rapid, effectively reduces broken glue residue, reaches the smooth row of returning and removes the purpose of shaft bottom hydrops.
The present invention does not have particular/special requirement to the preparation method of the fracturing fluid, using pressure well-known to those skilled in the art
The manner of formulation for splitting liquid is mixed each component in the fracturing fluid, for oil field compression fracture.
In the present invention, the preparation method of the fracturing fluid preferably includes following steps:
(I) the alcohol ether modified guar is dissolved in the water, obtains alcohol ether modified guar solution；
(II) by the obtained alcohol ether modified guar solution and the clay stabilizer, bactericide, Waterproof lock agent, alkali
Property pH value regulator and low temperature break the mixing of glue activator, obtain base fluid；
(III) the obtained base fluid and crosslinking agent, gel breaker are mixed, obtains fracturing fluid.
The present invention adjusts to the alcohol ether modified guar solution, clay stabilizer, bactericide, Waterproof lock agent, alkaline ph values
The embodiment for the mixing that section agent and low temperature break glue activator does not have particular/special requirement, can realize the uniform mixing of raw material
；The mixing is preferably carried out or carried out under condition of water bath heating at ambient temperature, and the heating water bath process helps
In the efficient progress of mixing；In an embodiment of the present invention, the mixing is specifically carried out in the mixed tune devices of Wu Yin.
After obtaining the base fluid, the base fluid and gel breaker, crosslinking agent are mixed to get fracturing fluid by the present invention.In the present invention
In, the fracturing fluid exists in the form of frozen glue.The present invention adds gel breaker, crosslinking agent preferably into the base fluid, is requiring
Base fluid crosslinks in time, obtains fracturing fluid gel.
The fracturing fluid gel is carried out heating water bath by the present invention, and after aquation occurs for frozen glue, the low temperature of mini-frac liquid is broken
Colloidality energy.
The preparation method and fracturing fluid of a kind of alcohol ether modified guar provided by the invention are carried out with reference to embodiment
Detailed description, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
0.1moL diglycols are dissolved in 50ml tetrahydrofurans (THF), obtain alcohol ether organic solution；Weigh simultaneously
0.2moL sodium hydroxides are dissolved in 50ml water, and 250ml three-necked flasks are poured into after alkali lye is mixed with alcohol ether organic solution, are being stirred
Under the conditions of carry out 10min ice-water bath.
Weigh paratoluensulfonyl chloride 0.1mol to be dissolved in 40mlTHF, constant pressure funnel is then fully transferred to, 0~5
Instill in the flask for completing ice-water bath, control drop speed, dripped off in 2 hours at DEG C.Continue reaction 2.5 hours after dripping off.
Mixture in flask is fully transferred in 100ml frozen water, uses CH2Cl2Extraction 2 times, separation lower floor oily liquids,
It is washed with water 2 times, then separates lower floor's oily liquids, with anhydrous MgSO4Dry, be evaporated after filtering, obtain the contracting diethyl two of product one
Alcohol single pair tosylate.
10g HPGs or Guar collagen powder are weighed, is evenly spread in 100ml THF, adds 0.1g hydroxides
Sodium, alkalize 0.5h under the conditions of 65 DEG C, obtains guar gum alkaline solution.
0.04mol sulfonation alcohol ethers are dissolved in 20ml THF and are fully transferred to constant pressure funnel, are slowly dropped into equipped with melon
In the flask of your glue alkaline solution, dripped off in 2h, continue at 63~66 DEG C after reacting 10h, filtered, then with absolute ethyl alcohol pair
Washing of Filter Cake three times, obtains alcohol ether modified guar.
Embodiment 2
0.1moL triethylene-glycols are dissolved in 50ml tetrahydrofurans (THF), obtain alcohol ether organic solution；Weigh simultaneously
0.2moL sodium hydroxides are dissolved in 50ml water, and 250ml three-necked flasks are poured into after alkali lye is mixed with alcohol ether organic solution, are being stirred
Under the conditions of carry out 20min ice-water bath.
Weigh paratoluensulfonyl chloride 0.1mol to be dissolved in 40mlTHF, constant pressure funnel is then fully transferred to, 0~5
Instill in the flask for completing ice-water bath, control drop speed, dripped off in 2 hours at DEG C.Continue reaction 2.5 hours after dripping off.
Mixture in flask is fully transferred in 100ml frozen water, uses CH2Cl2Extraction 2 times, separation lower floor oily liquids,
It is washed with water 2 times, then separates lower floor's oily liquids, with anhydrous MgSO4Dry, be evaporated after filtering, obtain three second two of contracting of product two
Alcohol single pair tosylate.
10g HPGs or Guar collagen powder are weighed, is evenly spread in 100ml THF, adds 0.1g hydroxides
Sodium, alkalize 0.5h under the conditions of 65 DEG C, obtains guar gum alkaline solution.
0.04mol sulfonation alcohol ethers are dissolved in 20ml THF and are fully transferred to constant pressure funnel, are slowly dropped into equipped with melon
In the flask of your glue alkaline solution, dripped off in 2h, continue at 63~66 DEG C after reacting 12h, filtered, then with absolute ethyl alcohol pair
Washing of Filter Cake three times, obtains alcohol ether modified guar.
Embodiment 3
The alcohol ether modified guar that 1.5g embodiments 1 are prepared is weighed, is dissolved in 490ml water, adds ammonium chloride 2.5g,
Chlorination benzalkonium 1g, the OPEO 1.5g of ten polyether units, the tetrahydroxy -2- of low-temp activation agent 2,3,5,6- oneself
Olefin(e) acid -4- lactone sodium 0.5g, pH adjusting agent sodium carbonate 0.35g, remaining is water.At room temperature in mixed 20 points of the stirrings in adjusting device of Wu Yin
Clock, then water-bath 1 hour in 30 DEG C of water-baths is placed in, it is fully swelled.1.5g crosslinking agents and 0.2g ammonium persulfates are added to
In the above-mentioned base fluid prepared, the preferable frozen glue of elasticity is formed, wherein crosslinking agent is the complex of Boratex and xylitol；
In the presence of pH value regulator, the pH value of fracturing fluid system reaches 9.2.
Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, carries out crush properties test.
Embodiment 4
The alcohol ether modified guar that 1.5g embodiments 2 are prepared is weighed, is dissolved in 490ml water, adds potassium chloride 2.5g,
Chlorination benzalkonium 1g, the NPE 1.5g of 12 polyether units, low-temp activation agent glucose and 2,3,5,6-
The mixture 0.5g of tetrahydroxy -2- hexenoic acid -4- lactone sodium, the sodium hydrate aqueous solution 0.35g of pH adjusting agent 20%, remaining is
Water.Stirred 20 minutes in the mixed tune devices of Wu Yin at room temperature, then be placed in water-bath 1 hour in 30 DEG C of water-baths, it is fully swelled.Will
1.5g crosslinking agents and 0.2g ammonium persulfates are added in the above-mentioned base fluid prepared, the preferable frozen glue of elasticity are formed, wherein being crosslinked
Agent is the complex of Boratex and glucose；In the presence of pH value regulator, the pH value of fracturing fluid system reaches 9.5.
Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, carries out crush properties test.
Embodiment 5
The alcohol ether modified guar that 1.51g embodiments 1 are prepared is weighed, is dissolved in 490ml water, adding molecular weight is
3000 Hydrin-Dodecyl Dimethyl Amine quaternary ammonium salt cationic polymer 2.52g, relative molecular weight 4500
The alkyl quaternary ammonium salts of daiamid-chlorination eight, the OPEO 1.51g of eight polyether units, citric acid and glucose
Mixture 0.53g, pH adjusting agent sodium carbonate 0.34g, remaining is water.Stirred 20 minutes in the mixed tune devices of Wu Yin at room temperature, then
Water-bath 1 hour in 30 DEG C of water-baths is placed in, it is fully swelled.1.53g crosslinking agents and 0.21g sodium peroxydisulfates are added to above-mentioned
In the base fluid prepared, the preferable frozen glue of elasticity is formed, wherein crosslinking agent is the ligand compound of sodium tetraborate and sodium gluconate
Thing；In the presence of pH value regulator, the pH value of fracturing fluid system reaches 9.0.
Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, carries out crush properties test.
Embodiment 6
The alcohol ether modified guar that 1.52g embodiments 2 are prepared is weighed, is dissolved in 490ml water, adding molecular weight is
The 3500 alkyl dimethyl tertiary amide quaternary ammonium salt cationic polymer 2.54g of Hydrin-eight, relative molecular weight are 4000
Daiamid-chlorination dodecyl quaternary ammonium salt 1.1g, the NPE 1.52g of ten polyether units, 2,3,5,6- tetra-
The mixture 0.53g of hydroxyl -2- hexenoic acids -4- lactones sodium and citric acid, the sodium hydrate aqueous solution 0.4g of pH adjusting agent 20%, its
Yu Weishui.Stirred 20 minutes in sterile mixed tune device at room temperature, then be placed in water-bath 1 hour in 30 DEG C of water-baths, make it fully molten
It is swollen.1.53g crosslinking agents and 0.22g sodium peroxydisulfates are added in the above-mentioned base fluid prepared, form the preferable frozen glue of elasticity, its
Middle crosslinking agent is hydration sodium tetraborate and the complex of xylitol；In the presence of pH value regulator, fracturing fluid system
PH value reaches 9.5.
Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, carries out crush properties test.
Comparative example 1:
The unmodified HPGs of 1.5g are weighed, are dissolved in 490ml water, add clay stabilizer 2.5g, bactericide
1g, Waterproof lock agent 1.5g, low-temp activation agent 0.5g, alkaline pH adjuster 0.35g, remaining is water.At room temperature in sterile mixed tune
Stirred 20 minutes in device, then be placed in water-bath 1 hour in 30 DEG C of water-baths.1.5g crosslinking agents and 0.2g ammonium persulfates are added to
State in the base fluid prepared, form the preferable frozen glue of elasticity.Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, entered
Row crush properties are tested.
Comparative example 2:
The unmodified Guar collagen powder of 1.5g is weighed, is dissolved in 490ml water, adds clay stabilizer 2.5g, bactericide 1g,
Waterproof lock agent 1.5g.Low-temp activation agent 0.5g, alkaline pH adjuster 0.35g, remaining is water.At room temperature in sterile mixed tune device
Stirring 20 minutes, then it is placed in water-bath 1 hour in 30 DEG C of water-baths.By 1.5g crosslinking agents and 0.2g ammonium persulfates be added to it is above-mentioned
In the base fluid prepared, the preferable frozen glue of elasticity is formed.Then frozen glue is placed in 30 DEG C of water-baths gradually broken glue, pressed
Split performance test.
According to standard SY/T5107-2005, the fracturing fluid prepared to embodiment 3 and 4 and comparative example 1 and 2 has carried out property
Can test.
The temperature and shearing sustainability testing result for the fracturing fluid that comparative example 1 is prepared, as shown in Figure 1；Embodiment 3 is made
The temperature and shearing sustainability testing result of standby obtained fracturing fluid, as shown in Figure 2.
From Fig. 1 and Fig. 2, for the fracturing fluid that comparative example 1 is prepared into after 50 DEG C of down cut 90min, viscosity keeps stable,
Viscosity is maintained at 90mPas or so；And the corresponding frozen glue for the fracturing fluid that embodiment 3 is prepared is in 50 DEG C of down cut 90min
Afterwards, viscosity keeps stable, and viscosity is maintained at 160mPas or so.It can be seen that modified guar fracturing fluid system provided by the invention
Frozen glue has good temperature and shearing sustainability.
Viscosity test results are as shown in table 1；And the solid-carrying performance of fracturing fluid and broken colloidality can be with the corresponding jellies of fracturing fluid
Glue form is detected, and it is as shown in table 2 to break glue the performance test results；Solid-carrying performance test result is as shown in table 3.
Temperature and shearing sustainability, method of testing referring to
The viscosity measurements result for the fracturing fluid that the embodiment 3~6 of table 1 and comparative example 1 and 2 obtain
From the data of table 1, the viscosity of modified guar fracturing fluid and the viscosity stabilization of unmodified Guar fracturing fluid
Property it is good, place 24h test after viscosity it is unchanged, it is seen that bactericide effectively inhibits decomposition of the bacterium to guar gum, simultaneously
It can be seen that modified guar stable performance.
The broken glue the performance test results for the fracturing fluid that the embodiment 3~6 of table 2 and comparative example 1 and comparative example 2 are prepared
As shown in Table 2, glue residue is broken after fracturing fluid aquation provided by the invention under 30 DEG C of cryogenic conditions to be respectively less than not
Broken glue level of residue after modified guar fracturing fluid aquation；Melon provided by the invention splits the minimum reachable 51mg of broken glue residue of liquid
L-1。
The solid-carrying performance test result for the fracturing fluid that the embodiment 3~5 of table 3 and comparative example 1 and comparative example 2 are prepared
As shown in Table 3, when the fracturing fluid that prepared by the present invention carries out taking sand, solid-carrying performance is superior to the pressure break that comparative example obtains
The sand carrying effect of the corresponding frozen glue of liquid；When the fracturing fluid that the present invention obtains carries out taking sand, 24h is can reach without sedimentation.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of alcohol ether modified guar, comprises the following steps：
(1) alcohol ether organic solution is mixed with strong base solution, carries out quaternization, obtain alcohol ether alkali；
(2) after paratoluensulfonyl chloride organic solution being added drop-wise to the alcohol ether alkali that the step (1) obtains, it is anti-to continue sulfonation
Should, obtain sulfonation alcohol ether；The speed of the dropwise addition is 20~32mL/h；
(3) after the organic solution for the sulfonation alcohol ether for obtaining the step (2) is added dropwise to the alkaline solution of guar gum, continue to connect
Branch reaction, obtains alcohol ether modified guar；The speed of the dropwise addition is 8~10mL/h.
2. preparation method according to claim 1, it is characterised in that in the step (1) temperature of quaternization be 0~
5 DEG C, the time of quaternization is 10~20min.
3. preparation method according to claim 1, it is characterised in that in the step (2) temperature of sulfonating reaction be 0~
5℃；The time of sulfonating reaction is 2.5~3h.
4. preparation method according to claim 1, it is characterised in that the temperature of graft reaction is 63 in the step (3)
~66 DEG C；The time of graft reaction is 10~12h.
5. a kind of fracturing fluid, include the component of following weight/mass percentage composition：Any one of Claims 1 to 4 preparation method system
Standby obtained alcohol ether modified guar 0.1~0.35%, clay stabilizer 0.1~0.3%, bactericide 0.1~0.2%, waterproof
Lock agent 0.25~0.3%, crosslinking agent 0.15~0.4%, gel breaker 0.04~0.06%, the broken glue activator 0.01 of low temperature~
0.03%, surplus is water and alkaline pH adjuster；
The dosage of the alkaline pH adjuster is defined by that can obtain the fracturing fluid that pH value is 8.5~12.
6. fracturing fluid according to claim 5, it is characterised in that the clay stabilizer is potassium chloride, ammonium chloride or phase
It is less than 5000 Polymeric quaternary ammonium salts to molecular weight.
7. fracturing fluid according to claim 5, it is characterised in that the crosslinking agent is organic boron complexes.
8. fracturing fluid according to claim 5, it is characterised in that the Waterproof lock agent is OPEO or nonyl
Base phenol polyethenoxy ether.
9. fracturing fluid according to claim 5, it is characterised in that the gel breaker is ammonium sulfate, potassium peroxydisulfate and over cure
One or more in sour ammonium.
10. the fracturing fluid according to claim 5 or 9, it is characterised in that the low temperature for activating the gel breaker breaks glue and swashed
Agent living is the one or more in glucose, 2,3,5,6- tetrahydroxys -2- hexenoic acids -4- lactones sodium and citric acid.
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| CN116083070A (en) * | 2023-02-23 | 2023-05-09 | 西安石油大学 | A kind of low-temperature jelly fracturing fluid and preparation method thereof |
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