CN103965390B - Polystyrene propping agent and preparation and application thereof - Google Patents
Polystyrene propping agent and preparation and application thereof Download PDFInfo
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- CN103965390B CN103965390B CN201410181659.1A CN201410181659A CN103965390B CN 103965390 B CN103965390 B CN 103965390B CN 201410181659 A CN201410181659 A CN 201410181659A CN 103965390 B CN103965390 B CN 103965390B
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- propping agent
- peroxide
- initiator
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 65
- 239000004793 Polystyrene Substances 0.000 title claims abstract description 24
- 229920002223 polystyrene Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003999 initiator Substances 0.000 claims abstract description 27
- 239000000178 monomer Substances 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 15
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 15
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 13
- -1 alkoxy rare-earth Chemical class 0.000 claims description 13
- 238000005728 strengthening Methods 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- 239000004159 Potassium persulphate Substances 0.000 claims description 8
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 235000019394 potassium persulphate Nutrition 0.000 claims description 8
- 108010010803 Gelatin Proteins 0.000 claims description 7
- 239000013543 active substance Substances 0.000 claims description 7
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 239000001506 calcium phosphate Substances 0.000 claims description 7
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 7
- 235000011010 calcium phosphates Nutrition 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000008273 gelatin Substances 0.000 claims description 7
- 229920000159 gelatin Polymers 0.000 claims description 7
- 235000019322 gelatine Nutrition 0.000 claims description 7
- 235000011852 gelatine desserts Nutrition 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000004005 microsphere Substances 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 7
- 238000003828 vacuum filtration Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000004160 Ammonium persulphate Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical group CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 claims description 4
- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005553 drilling Methods 0.000 claims description 4
- 239000012934 organic peroxide initiator Substances 0.000 claims description 4
- 230000033116 oxidation-reduction process Effects 0.000 claims description 4
- 238000005502 peroxidation Methods 0.000 claims description 4
- 150000002978 peroxides Chemical class 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 3
- 239000003456 ion exchange resin Substances 0.000 claims description 3
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 2
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 claims description 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical group CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- ATEAWHILRRXHPW-UHFFFAOYSA-J iron(2+);phosphonato phosphate Chemical compound [Fe+2].[Fe+2].[O-]P([O-])(=O)OP([O-])([O-])=O ATEAWHILRRXHPW-UHFFFAOYSA-J 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 125000002510 isobutoxy group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])O* 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 125000005921 isopentoxy group Chemical group 0.000 claims description 2
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 claims description 2
- 125000005447 octyloxy 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])O* 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 2
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical group CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229960001866 silicon dioxide Drugs 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 229940095064 tartrate Drugs 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000000230 xanthan gum Substances 0.000 claims 1
- 229920001285 xanthan gum Polymers 0.000 claims 1
- 229940082509 xanthan gum Drugs 0.000 claims 1
- 235000010493 xanthan gum Nutrition 0.000 claims 1
- 229920000620 organic polymer Polymers 0.000 abstract description 9
- 239000004094 surface-active agent Substances 0.000 abstract description 6
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000005484 gravity Effects 0.000 abstract 1
- 239000012744 reinforcing agent Substances 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 6
- 150000001721 carbon Chemical class 0.000 description 6
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000010907 mechanical stirring Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 3
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical group C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- WYJPHIFPHKRGPP-UHFFFAOYSA-N C(C(C)C)O[Ho] Chemical compound C(C(C)C)O[Ho] WYJPHIFPHKRGPP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- NWZPZAQIKFZIOP-UHFFFAOYSA-N C(C)(C)O[Pr] Chemical compound C(C)(C)O[Pr] NWZPZAQIKFZIOP-UHFFFAOYSA-N 0.000 description 1
- YUYXETVVDDGZJC-UHFFFAOYSA-N CC(C)CO[Eu] Chemical compound CC(C)CO[Eu] YUYXETVVDDGZJC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003190 augmentative effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of organic polymer materials, in particular to a polystyrene propping agent and a preparation and application thereof. The invention aims to provide the polystyrene organic polymer propping agent which can achieve the purpose of increasing oil-gas well output and prolonging oil-gas well fracturing usable life through changing the composition of the propping agent. The propping agent comprises the following components in parts by weight: 100 parts of monomer, 0.11-8 parts of an initiator, 2-10 parts of an inorganic dispersing agent, 2-7 parts of an organic dispersing agent, 0.2-1 part of a reinforcing agent, 200-500 parts of deionized water, and 0.8-3 parts of a surface active agent, wherein the monomer is phenethylene or a mixture of phenethylene and divinylbenzene. The polystyrene propping has the advantages of low specific gravity, no electrostatic, less probability of smashing, low cost, no pollution and the like.
Description
Technical field
The present invention relates to organic polymer material field, particularly a kind of polystyrene propping agent and its preparation method and application.
Background technology
At present in oil/gas drilling field, fracturing technique is widely adopted.Fracturing technique is not only widely used in Low permeable oil and gas reservoirs, and also achieves effect clearly in the storey increase design of middle and high penetrating oil gas reservoir.Be exactly after drilling by injecting high pressure fluid in well, high pressure has been suppressed in shaft bottom, when this pressure is greater than terrestrial stress and the formation rock tensile strength of Around A Borehole, stratum generation crack near shaft bottom, continue to inject the liquid with propping agent, crack extends forward and fills out with propping agent, after closing well, crack closure is on propping agent, thus stratum is formed and has the crack being filled with propping agent of certain geometrical dimension and flow conductivity near shaft bottom, Oil/gas Well is made to reach the object in volume increase, augmented injection and prolongation Oil/gas Well secondary or repeatedly pressure break cycle.Traditional propping agent is inorganics or its coatings such as glass sphere, Metal Ball, quartz sand, haydite, the following shortcoming of these propping agent ubiquities: 1, than great, all more than 2.0, when causing transmitting propping agent in fracturing process, fluid viscosity is large, pump pressure is high, energy consumption is large; 2, circularity and sphericity low, rough, to the serious wear of equipment; 3, easily broken, cause crack to close too early, affect output; 4, there is overlay film on surface, easily produces adhesion, causes line clogging.
Summary of the invention
A kind of composition by changing propping agent is the object of the present invention is to provide to reach the polystyrene organic polymer propping agent improving oil gas well yield and extend well fracturing validity period.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of polystyrene propping agent, is characterized in that, comprise according to mass fraction: 100 parts of monomers, 0.11-8 part initiator, 2-10 part inorganic dispersant, 2-7 part organic dispersing agent, 0.2-1 part strengthening agent, 200-500 part deionized waters; Described monomer is styrene-divinylbenzene mixed solution.Described monomer is vinylbenzene or styrene-divinylbenzene mixture, and preferably, linking agent divinylbenzene is the 0-60% of vinylbenzene quality.
Described propping agent can also comprise 0.01-5 part toughner.
Described initiator is organic peroxide initiator, inorganic peroxide class initiator, from azo-initiator, and one or more of oxidation-reduction class initiator.
Preferably, described organic peroxide initiator comprises in Cumene Hydroperoxide 80, hydroperoxidation tertiary butyl, dibenzoyl peroxide, dilauroyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, di-isopropyl peroxydicarbonate.
Described inorganic peroxide class initiator comprises Potassium Persulphate, Sodium Persulfate, ammonium persulphate;
Describedly comprise Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) from azo-initiator;
What described oxidation-reduction class initiator comprised redox system has benzoyl peroxide/sucrose, tertbutyl peroxide/rongalite, tertbutyl peroxide/Sodium Pyrosulfite, benzoyl peroxide/DMA.Ammonium persulphate/sodium bisulfite, Potassium Persulphate/sodium bisulfite, hydrogen peroxide/tartrate, hydrogen peroxide/rongalite, ammonium persulphate/ferrous sulfate, hydrogen peroxide/sulfuric acid are ferrous, benzoyl peroxide //N, N-Diethyl Aniline, benzoyl peroxide/ferrous pyrophosphate, Potassium Persulphate/Silver Nitrate, persulphate/mercaptan, isopropyl benzene hydroperoxide/iron protochloride, Potassium Persulphate/iron protochloride, hydrogen peroxide/iron protochloride, isopropyl benzene hydroperoxide/tetra-ethyleneimine etc.
More preferably, described initiator is benzoyl peroxide and/or peroxidation (2-ethyl) the caproic acid tertiary butyl.
Preferably, described inorganic dispersant is anhydrous sodium sulphate, active calcium phosphate, talcous one or more; Be more preferably active calcium phosphate;
Preferably, described organic dispersing agent is polyvinyl alcohol, gelatin, Walocel MT 20.000PV, one or more of Polyvinylpyrolidone (PVP); Be more preferably gelatin;
Preferably, described strengthening agent adopts carbon black, or has cancellated inorganics, as silicon-dioxide, and norbide, white carbon black etc.;
Preferably, described tensio-active agent is Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, sodium lauryl sulphate, Sionit acid anhydride oleic acid ester, one or more in alkylphenol polyoxyethylene or nonionogenic tenside polyoxyethylene nonylphenol ether.
Preferably, described toughner is one or two or more kinds in alkoxy rare-earth; Alkoxyl group is three isopropoxies, three isobutoxies, three isopentyloxy or three different octyloxies; Described rare earth is holmium, praseodymium, europium, gadolinium, terbium, dysprosium or erbium.
The preferred ball-type solid of gained propping agent finished product, preferably diameter is the ball-type solid of 0.1--4.0mm further; Propping agent can be white, black or other color; This color is according to adding different strengthening agent changes.
The preparation method of described propping agent, comprises the steps:
1) pre-treatment of strengthening agent:
Tensio-active agent: the mass ratio mixing of deionized water=1:5-1:30-50,80-90 DEG C is stirred 8-12h, vacuum filtration washed several times with water, filters to the packed sealing of mud cake shape and saves backup;
2) preparation of crosslinked polystyrene microsphere: add tensio-active agent in a kettle., deionized water, inorganic dispersant, stir evenly; By step 1) add in reactor after gained strengthening agent and deionized water ultrasonic disperse and stir well; Stirring well adding in reactor after initiator and monomer mixing again, making strengthening agent enter monomer by aqueous phase; Slowly be warming up to 70-80 DEG C, add inorganic dispersant; 90-100 DEG C of insulation 5-8h; Washing after being released by material, solid-liquid separation, drying, screening, namely obtains polystyrene propping agent.
Described propping agent is applied in oil/gas drilling fracturing process as propping agent, the locking pressure that is greater than 170Mpa can be born or as ion exchange resin or support applications in other aspects.
The invention has the advantages that:
1. proportion is low, between 0.9-1.2, is organic synthesis, because propping agent is carried by liquid, is sent to shaft bottom through high-pressure pump.If than great, just high to the requirement of carrying propping agent liquid, otherwise propping agent just easy precipitation, cost is just high, and pump certainly will need higher pressure in the process of transmission simultaneously, and energy expenditure is huge;
2. circularity and sphericity high, smooth surface, propping agent of the present invention is perfectly smooth spheroid, does not have corner angle, reduces the wearing and tearing to equipment;
3. be insoluble to acid, alkali, oil, water, without electrostatic so there is no inter-adhesive situation, there will not be early stage adhesion blocking pipe;
4. normal polystyrene system microballoon all adopts vinylbenzene and divinyl benzene crosslinked to react at present, take benzoyl peroxide as initiator, polyvinyl alcohol is that dispersion agent carries out suspension polymerization, its product high temperature resistance and crushing resistance all lower, this product excellent heat stability, more than 245 degrees Celsius can be reached, not easily broken, the locking pressure that general fracturing propping agents are the highest is 100MPa, the anti-locking pressure of propping agent provided by the invention can reach more than 170MPa, far away higher than the specified requirement of SY/T5108--2006;
5. temperature of reaction is lower, works at ambient pressure, and technique is simple, and cost is lower, is applicable to large-scale commercial production;
6. nontoxic, environment is safe from harm;
7. this product applied range, except for except propping agent, also can be used for but is not limited to as ion exchange resin, support of the catalyst etc.
Embodiment
Embodiment 1:
Carbon black modified: by carbon black 4g, Sodium dodecylbenzene sulfonate 8g, deionized water 200g mix, and 80 DEG C are stirred 8h, vacuum filtration washed several times with water, filter to the packed sealing of mud cake shape and save backup.
The preparation of black crosslinked polystyrene microsphere: add surfactant sodium dodecyl base benzene sulfonic acid sodium salt 2.8g in a kettle., deionized water 400mL, inorganic dispersant active calcium phosphate 7g, mechanical stirring 20min, speed 160rpm.By modified carbon black 1g and deionized water 40mL, ultrasonic disperse 60min, add in reactor, stir 60min.By initiator benzoyl peroxide 2g, vinylbenzene 90g, divinylbenzene 10g, add after mixing in reactor, keep speed 160rpm to stir 10min, make modified carbon black enter monomer by aqueous phase.In 1.5h, be slowly warming up to 75 DEG C, along with temperature rises, monomer is initiated polymerization, and monomer viscosity rises gradually, adds gelatin solution 50mL, stirs speedup to 250rpm.95 DEG C of insulation 6h.Washing after being released by material, solid-liquid separation, drying, screening, namely obtains crosslinked polystyrene organic polymer propping agent.
After testing, product indices is as follows: proportion: 0.9--1.2g/cm
3ultimate compression strength>=60N, (ultimate compression strength is individual attribute to locking pressure>=170MPa, locking pressure is the ability that entirety embodies), thermostability>=245 DEG C, particle diameter: 0.4--1.2mm, acid solubility <4.0%, percentage of damage <3.0%, sphericity and circularity>=0.95.
Embodiment 2:
Carbon black modified: by carbon black 4g, Sodium dodecylbenzene sulfonate 6g, deionized water 220g mix, and 80 DEG C are stirred 8h, vacuum filtration washed several times with water, filter to the packed sealing of mud cake shape and save backup.
The preparation of black crosslinked polystyrene microsphere: add surfactant sodium dodecyl base benzene sulfonic acid sodium salt 2.5g in a kettle., deionized water 350mL, inorganic dispersant active calcium phosphate 6g, mechanical stirring 20min, speed 170rpm.By modified carbon black 0.8g and deionized water 40mL, ultrasonic disperse 50min, add in reactor, stir 60min.By initiator peroxidation (2-ethyl) caproic acid tertiary butyl 1.6g, vinylbenzene 92g, divinylbenzene 8g, toughner three isopropoxy praseodymium 3g, adds after mixing in reactor, keeps speed 170rpm to stir 10min, makes modified carbon black enter monomer by aqueous phase.In 1.5h, be slowly warming up to 72 DEG C, along with temperature rises, monomer is initiated polymerization, and monomer viscosity rises gradually, adds gelatin solution 55mL, 95 DEG C of insulation 6h.Washing after being released by material, solid-liquid separation, drying, screening, namely obtains crosslinked polystyrene organic polymer propping agent.
After testing, product indices is as follows: proportion: 0.9--1.2g/cm
3, ultimate compression strength>=60N, locking pressure>=170MPa, thermostability>=245 DEG C, particle diameter: 0.3--1.2mm, acid solubility <4.0%, percentage of damage <3.0%, sphericity and circularity>=0.95.
Embodiment 3:
Carbon black modified: by carbon black 4g, Sodium dodecylbenzene sulfonate 6g, deionized water 180g mix, and 90 DEG C are stirred 9h, vacuum filtration washed several times with water, filter to the packed sealing of mud cake shape and save backup.
The preparation of black crosslinked polystyrene microsphere: add surfactant sodium dodecyl base benzene sulfonic acid sodium salt 1.3g in a kettle., deionized water 300mL, inorganic dispersant active calcium phosphate 4g, mechanical stirring 20min, speed 200rpm.By modified carbon black 0.2g and deionized water 20mL, ultrasonic disperse 60min, add in reactor, stir 40min.By initiator benzoyl peroxide and peroxidation (2-ethyl) caproic acid tertiary butyl mixture 1.2g, vinylbenzene 96g, divinylbenzene 4g, toughner three isobutoxy holmium 3g, add after mixing in reactor, keep speed 200rpm to stir 20min, make modified carbon black enter monomer by aqueous phase.In 1.5h, be slowly warming up to 73 DEG C, along with temperature rises, monomer is initiated polymerization, and monomer viscosity rises gradually, adds gelatin solution 50mL.90 DEG C of insulation 8h.Washing after material is released, solid-liquid separation, drying, screening, namely obtains crosslinked polystyrene organic polymer propping agent.
After testing, product indices is as follows: proportion: 0.9--1.2g/cm
3, ultimate compression strength>=60N, locking pressure>=170MPa, thermostability>=245 DEG C, particle diameter: 0.1--1.2mm, acid solubility <4.0%, percentage of damage <3.0%, sphericity and circularity>=0.95.
Embodiment 4:
White carbon black modification: by white carbon black 4g, sodium laurylsulfonate 6g, deionized water 180g mix, and 90 DEG C are stirred 9h, vacuum filtration washed several times with water, filter to the packed sealing of mud cake shape and save backup.
The preparation of white crosslinked polystyrene microsphere: add surfactant sodium dodecyl base sodium sulfonate 1.3g in a kettle., deionized water 300mL, inorganic dispersant talcum powder 4g, mechanical stirring 20min, speed 200rpm.By modified white carbon black 0.2g and deionized water 20mL, ultrasonic disperse 60min, add in reactor, stir 40min.By initiator potassium persulfate 0.2g, vinylbenzene 96g, divinylbenzene 4g, toughner three isobutoxy europium 2g, adds after mixing in reactor, keeps speed 200rpm to stir 20min, makes modified white carbon black enter monomer by aqueous phase.In 1.5h, be slowly warming up to 73 DEG C, along with temperature rises, monomer is initiated polymerization, and monomer viscosity rises gradually, adds polyvinyl alcohol solution 50mL.100 DEG C of insulation 5h.Washing after being released by material, solid-liquid separation, drying, screening, namely obtains crosslinked polystyrene organic polymer propping agent.
After testing, product indices is as follows: proportion: 0.9--1.2g/cm
3, ultimate compression strength>=60N, locking pressure>=170MPa, thermostability>=245 DEG C, particle diameter: 0.1--1.2mm, acid solubility <4.0%, percentage of damage <3.0%, sphericity and circularity>=0.95.
Embodiment 5:
Norbide and carbon black modified: by norbide 2g and carbon black 2g, sodium lauryl sulphate 8g, deionized water 200g mixes, 80 DEG C are stirred 8h, vacuum filtration washed several times with water, filter to the packed sealing of mud cake shape and save backup.
The preparation of black crosslinked polystyrene microsphere: add Surfactant SDS 2.8g in a kettle., deionized water 400mL, inorganic dispersant active calcium phosphate and each 3.5g of anhydrous sodium sulphate, mechanical stirring 20min, speed 160rpm.By modified carbonize boron and each 0.5g of carbon black and deionized water 40mL, ultrasonic disperse 60min, add in reactor, stir 60min.By initiator 8g, vinylbenzene 90g, divinylbenzene 10g, toughner three isobutoxy holmium 5g, adds after mixing in reactor, keeps speed 160rpm to stir 10min, makes modified carbonize boron and carbon black enter monomer by aqueous phase.In 1.5h, be slowly warming up to 75 DEG C, along with temperature rises, monomer is initiated polymerization, and monomer viscosity rises gradually, adds gelatin solution 50mL, stirs speedup to 250rpm.95 DEG C of insulation 6h.Washing after material is released, solid-liquid separation, drying, screening, namely obtains crosslinked polystyrene organic polymer propping agent.
After testing, product indices is as follows: proportion: 0.9--1.2g/cm
3, ultimate compression strength>=60N, locking pressure>=170MPa, thermostability>=245 DEG C, particle diameter: 0.4--1.2mm, acid solubility <4.0%, percentage of damage <3.0%, sphericity and circularity>=0.95.
Detection method of the present invention and data are with reference to People's Republic of China's oil and gas industry standard " fracturing propping agents performance index and test recommend method " SY/T5108--2006.
Claims (10)
1. a polystyrene propping agent, it is characterized in that, according to mass fraction, raw material comprises: 100 parts of monomers, 0.11-8 part initiator, 2-10 part inorganic dispersant, 2-7 part organic dispersing agent, 0.2-1 part strengthening agent, 200-500 part deionized water, 0.8-3 part tensio-active agents; Described monomer is the mixture of vinylbenzene and divinylbenzene; In described monomer, the quality of divinylbenzene is less than or equal to 60% of vinylbenzene quality, but is not equal to zero; 0.01-5 part toughner is also included in propping agent composition.
2. propping agent according to claim 1, is characterized in that, described toughner is one or two or more kinds in alkoxy rare-earth; Alkoxyl group is three isopropoxies, three isobutoxies, three isopentyloxy or three different octyloxies; Described rare earth is holmium, praseodymium, europium, gadolinium, terbium, dysprosium or erbium.
3. propping agent according to claim 1 and 2, is characterized in that, described initiator is organic peroxide initiator, inorganic peroxide class initiator, one or two or more kinds from azo-initiator, in oxidation-reduction class initiator.
4. propping agent according to claim 3, it is characterized in that, described organic peroxide initiator comprises one or two or more kinds in Cumene Hydroperoxide 80, hydroperoxidation tertiary butyl, dibenzoyl peroxide, dilauroyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, di-isopropyl peroxydicarbonate;
Described inorganic peroxide class initiator comprises one or two or more kinds in Potassium Persulphate, Sodium Persulfate, ammonium persulphate;
Described from azo-initiator comprise in Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) one or two or more kinds;
What described oxidation-reduction class initiator comprised redox system has benzoyl peroxide/sucrose, tertbutyl peroxide/rongalite, tertbutyl peroxide/Sodium Pyrosulfite, benzoyl peroxide/DMA.One or two or more kinds in ammonium persulphate/sodium bisulfite, Potassium Persulphate/sodium bisulfite, hydrogen peroxide/tartrate, hydrogen peroxide/rongalite, ammonium persulphate/ferrous sulfate, hydrogen peroxide/sulfuric acid ferrous iron, benzoyl peroxide //N, N-Diethyl Aniline, benzoyl peroxide/ferrous pyrophosphate, Potassium Persulphate/Silver Nitrate, persulphate/mercaptan, isopropyl benzene hydroperoxide/iron protochloride, Potassium Persulphate/iron protochloride, hydrogen peroxide/iron protochloride, isopropyl benzene hydroperoxide/tetra-ethyleneimine.
5. propping agent according to claim 3, is characterized in that, described initiator is benzoyl peroxide and/or peroxidation (2-ethyl) the caproic acid tertiary butyl.
6. propping agent according to claim 1 and 2, is characterized in that, described inorganic dispersant is anhydrous sodium sulphate, active calcium phosphate, one or two or more kinds in talcum powder; Described organic dispersing agent is xanthan gum, polyvinyl alcohol, gelatin, Walocel MT 20.000PV, Natvosol, one or two or more kinds in Polyvinylpyrolidone (PVP).
7. propping agent according to claim 1 and 2, is characterized in that, described strengthening agent is one or two or more kinds in carbon black, white carbon black, silicon-dioxide or norbide; Described tensio-active agent is Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, sodium lauryl sulphate, Sionit acid anhydride oleic acid ester,, one or two or more kinds in alkylphenol polyoxyethylene or nonionogenic tenside polyoxyethylene nonylphenol ether.
8. propping agent according to claim 1 and 2, is characterized in that, described propping agent obtains the preferred ball-type solid of finished product.
9. a preparation method for the arbitrary described propping agent of claim 1-8, is characterized in that, comprise the steps:
1) pre-treatment of strengthening agent:
Strengthening agent: tensio-active agent: the mass ratio mixing of deionized water=1:5-1:30-50,80-90 DEG C is stirred 8-12h, vacuum filtration washed several times with water, filters to the packed sealing of mud cake shape and saves backup;
2) preparation of crosslinked polystyrene microsphere: add tensio-active agent in a kettle., deionized water, inorganic dispersant, stir evenly; By step 1) add in reactor after gained strengthening agent and deionized water ultrasonic disperse and stir well; Add in reactor after again initiator, toughner and monomer being mixed and stir well, make strengthening agent enter monomer by aqueous phase; Slowly be warming up to 70-80 DEG C, add inorganic dispersant; 90-100 DEG C of insulation 5-8h; Washing after being released by material, solid-liquid separation, drying, screening, namely obtains polystyrene propping agent.
10. the arbitrary described propping agent of claim 1-8 is as the application of propping agent in oil/gas drilling fracturing process, or as the application of ion exchange resin or support of the catalyst aspect.
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| CN106701055A (en) * | 2016-12-27 | 2017-05-24 | 常州大学 | Preparation method of lightweight and high-strength fracturing propping agent |
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| CN114874762B (en) * | 2022-05-18 | 2023-05-09 | 西安博众科技发展有限责任公司 | Polystyrene composite fracturing propping agent and preparation method thereof |
| CN115746192A (en) * | 2022-12-31 | 2023-03-07 | 西南石油大学 | Low-density high-strength proppant and preparation method thereof |
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| CN100558809C (en) * | 2005-12-29 | 2009-11-11 | 中国石油化工股份有限公司 | A kind of preparation method of organic-inorganic composite material |
| US8006754B2 (en) * | 2008-04-05 | 2011-08-30 | Sun Drilling Products Corporation | Proppants containing dispersed piezoelectric or magnetostrictive fillers or mixtures thereof, to enable proppant tracking and monitoring in a downhole environment |
| CN103387681B (en) * | 2012-05-07 | 2015-09-09 | 中国石油化工股份有限公司 | The preparation method of polystyrene plastic pellet and application thereof |
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Effective date of registration: 20231219 Address after: Room 601, No. 9 Chenggong Road, Dandong City, Liaoning Province, 118000 Patentee after: Wang Wenjun Patentee after: Shi Yong Patentee after: Guo Chengzhen Patentee after: Wang Chunyan Patentee after: Wang Xiuhong Patentee after: HEBEI HUAYUN HONGYE CHEMICAL INDUSTRY Co.,Ltd. Address before: Room 601, No. 9 Chenggong Road, Dandong City, Liaoning Province, 118000 Patentee before: Wang Wenjun Patentee before: Shi Yong Patentee before: Guo Chengzhen Patentee before: Wang Chunyan Patentee before: Wang Xiuhong |