CN114774102B - Degradable rope knot type temporary plugging agent for fracturing and preparation method thereof - Google Patents
Degradable rope knot type temporary plugging agent for fracturing and preparation method thereof Download PDFInfo
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- CN114774102B CN114774102B CN202210704007.6A CN202210704007A CN114774102B CN 114774102 B CN114774102 B CN 114774102B CN 202210704007 A CN202210704007 A CN 202210704007A CN 114774102 B CN114774102 B CN 114774102B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 200
- 238000009987 spinning Methods 0.000 claims abstract description 39
- 238000009941 weaving Methods 0.000 claims abstract description 37
- 238000002074 melt spinning Methods 0.000 claims abstract description 34
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 238000004804 winding Methods 0.000 claims abstract description 23
- PVJDYCWESWOLKI-UHFFFAOYSA-N C(C=C)(=O)O.C(C=C)(=O)O.C(C=C)(=O)O.C(O)C(CC)(CO)CO.OCC(O)CO Chemical compound C(C=C)(=O)O.C(C=C)(=O)O.C(C=C)(=O)O.C(O)C(CC)(CO)CO.OCC(O)CO PVJDYCWESWOLKI-UHFFFAOYSA-N 0.000 claims abstract description 21
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 16
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 16
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 16
- WIRIPVDRZYVTCG-UHFFFAOYSA-N dimethyl-prop-2-enyl-pyridin-2-ylsilane Chemical compound C=CC[Si](C)(C)C1=CC=CC=N1 WIRIPVDRZYVTCG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- TZYULTYGSBAILI-UHFFFAOYSA-M trimethyl(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC=C TZYULTYGSBAILI-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 239000000839 emulsion Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229920000642 polymer Polymers 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 14
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 14
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 12
- 238000010926 purge Methods 0.000 claims description 11
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 6
- 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 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- 238000011084 recovery Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 17
- 230000000903 blocking effect Effects 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- 239000007789 gas Substances 0.000 description 8
- 230000035699 permeability Effects 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000010276 construction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- -1 polyoxyethylene Polymers 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- VFDYEMVVNIPATA-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;propane-1,2,3-triol Chemical compound OCC(O)CO.CCC(CO)(CO)CO VFDYEMVVNIPATA-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- BZUOCSHAJKFNRJ-UHFFFAOYSA-N 3-(2,3-dihydroxypropoxy)propane-1,1,1-triol Chemical compound OCC(O)COCCC(O)(O)O BZUOCSHAJKFNRJ-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- 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
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- C09K8/62—Compositions for forming crevices or fractures
- C09K8/70—Compositions for forming crevices or fractures characterised by their form or by the form of their components, e.g. foams
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04C—BRAIDING OR MANUFACTURE OF LACE, INCLUDING BOBBIN-NET OR CARBONISED LACE; BRAIDING MACHINES; BRAID; LACE
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- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
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Abstract
The invention belongs to the technical field of tertiary oil recovery, and particularly relates to a degradable rope knot type temporary plugging agent for fracturing and a preparation method thereof. The degradable rope knot type temporary plugging agent is prepared by taking glycerol trimethylolpropane triacrylate, 2- (allyl dimethyl silyl) pyridine, 1-vinyl-2-pyrrolidone, allyl alcohol polyoxyethylene ether and allyl trimethyl ammonium chloride as raw materials to obtain temporary plugging agent particles; drying, melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; spinning the temporary plugging agent to generate a temporary plugging agent composite thread; weaving the composite thread to produce a temporary plugging agent thread end; then weaving the temporary plugging agent thread ends into temporary plugging agent ropes; finally drying to prepare the degradable rope knot type temporary plugging agent for fracturing. The invention adopts six steps of synthesis, melting, spinning, weaving, cutting and drying to directly obtain the finished product, and the preparation method is simple and easy to operate, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the technical field of tertiary oil recovery, relates to a high molecular polymer and a preparation method thereof, and particularly relates to a degradable rope knot type temporary plugging agent for fracturing and a preparation method thereof.
Background
At present, unconventional oil and gas exploitation such as low-permeability hard-to-use reserves, shale oil and gas, dense oil and gas and the like are increasingly becoming main objects of development. The fracturing and acidizing reservoir reformation technology is a main means for exploiting the unconventional oil and gas reservoirs, and the staged fracturing and acidizing reformation technology is a necessary way for realizing the targeted reformation of the reservoir.
The prior art of implementing the staged reforming is generally divided into mechanical and chemical methods. The common tool in the mechanical method is a packer or a bridge plug, on one hand, the product is expensive, sand blocking accidents are easily caused in the construction process, overhaul is needed, overhaul fails, and the well is often scrapped, and on the other hand, an effective mechanical packer tool cannot be put into the well with casing deformation. The temporary plugging agent is commonly used in a chemical method, the temporary plugging agent commonly used in the oil field at present is fiber and water-soluble particles with different sizes, wherein the most widely used temporary plugging agent is polymer and plugging pellets, the temporary plugging agent of the polymer has a good plugging effect due to a firm chemical cross-linked network structure, but has the phenomenon of slow gel breaking or even difficult gel breaking, the flowback is not thorough, the temporary plugging agent of the polymer can cause certain damage to a stratum, the temperature resistance of the temporary plugging agent of the polymer is low, the dissolution time is not well controlled, and the temporary plugging agent of the polymer is only suitable for oil and gas wells with shallow buried depth and low bottom temperature; the plugging small ball has the characteristics of high plugging strength and small deformation, is easy to fall off when applied in a straight well, has poor plugging effect, is easy to form accumulation in a horizontal section shaft when applied in a horizontal well, and cannot effectively plug the upper hole of the horizontal section; meanwhile, the degradation performance of the temporary plugging agent is related to whether the temporary plugging agent can effectively plug cracks and realize plugging removal. If the degradability of the temporary plugging agent is poor, after fracturing construction is finished, the temporary plugging agent cannot be degraded quickly, and is filled between propping agents for a long time to prevent oil and gas from normally permeating, so that the fracturing purpose can be achieved, but the yield of an oil field and a gas field cannot be increased, and the yield is influenced. The degradable temporary plugging agent is more and more emphasized due to the characteristics of environmental protection, no pollution, self cleaning and small formation damage.
CN108300439A discloses a water-soluble temporary plugging agent for oil-gas well fracturing temporary plugging steering, which consists of the following components: unsaturated organic acid, sodium methallyl sulfonate, N-vinyl pyrrolidone, polyoxyethylene allyl ester, an initiator, sodium hydroxide, a nano modifier and distilled water. The preparation method comprises the following steps: firstly, adding distilled water into a reaction container, and introducing nitrogen to replace air; then adding unsaturated organic acid, sodium methallyl sulfonate and N-vinyl pyrrolidone into a reaction vessel, stirring, adding 1/2 initiator, heating to 110 ℃, reacting for 30min, and adding sodium hydroxide; and then heating the reaction solution to 145-155 ℃, reacting for 1.0h, adding polyoxyethylene allyl ester and an initiator, heating to 175-185 ℃, adding the remaining 1/2 initiator, reacting for 2h, adding a modifier, and drying to obtain the product. The temporary plugging agent has good temporary plugging steering effect and little damage to the stratum after degradation.
CN105441050A 'A functional bridging particle temporary plugging agent and its preparation method', the functional bridging particle temporary plugging agent can automatically adjust the structure or shape, rapidly bridge in a leakage passage, occupy the reservoir storage and seepage space to the maximum extent, and form temporary plugging. Another invention patent application CN103615228A 'temporary plugging fracturing process in degradable fiber seam' refers to a degradable fiber and linear glue and proppant as temporary plugging fracturing fluid in the seam to form a branch seam.
The temporary plugging technology is basically based on friction accumulation (or bridging enrichment) of temporary plugging particles or fibers in a seam or a seam opening (blasthole) to form a bridge plug, the accumulation or enrichment is a fuzzy process, the temporary plugging time and position cannot be determined, the thickness of the temporary plug formed through accumulation cannot be determined due to the loss of a temporary plugging agent, the strength and the effect of the temporary plug cannot be guaranteed, and the subsequent crack opening of a new seam is influenced. In addition, the conventional temporary plugging fracturing technology basically determines the adding amount of the temporary plugging agent according to the change of the construction pressure on the ground, so that the temporary plugging agent needs to be prepared in advance on the ground, and waste is caused. Meanwhile, the degradation time cannot be controlled, heavy metals are contained in the formula, and the flowback liquid has the problem of environmental damage.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a degradable rope knot type temporary plugging agent for fracturing and a preparation method thereof. The invention adopts six steps of synthesis, melting, spinning, weaving, cutting and drying to directly obtain the finished product, and the preparation method is simple and easy to operate, and is beneficial to industrial production.
In order to achieve the purpose, one of the purposes of the invention discloses a preparation method of a degradable rope knot type temporary plugging agent for fracturing, which comprises the following specific steps:
(1) purging the reactor for 2-3min by nitrogen, sequentially adding glycerol trimethylolpropane triacrylate, 2- (allyl dimethyl silyl) pyridine, 1-vinyl-2-pyrrolidone, allyl alcohol polyoxyethylene ether, allyl trimethyl ammonium chloride, span 60, sodium dodecyl sulfate and water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 40-45 ℃, slowly dripping an initiator solution into the elevated tank, dripping a reducing agent solution into the elevated tank, wherein in the dripping process, the reaction releases heat, the temperature is automatically increased, and after finishing dripping, heating to 60-65 ℃, continuously stirring for 2-3h, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
(4) weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; and then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, and drying to prepare the degradable rope knot type temporary plugging agent for fracturing.
In the present invention, it is preferable that the 2- (allyldimethylsilyl) pyridine, the 1-vinyl-2-pyrrolidone, the allylalcohol polyoxyethylene ether, and the allyltrimethylammonium chloride are used in an amount of 0.5 to 5 parts by mole, 0.2 to 5 parts by mole, and 0.2 to 2 parts by mole, respectively, based on 1 part by mole of glycerol trimethylolpropane triacrylate.
Preferably, in the step (1), the weight ratio of span 60, sodium lauryl sulfate, water and glycerol trimethylolpropane triacrylate is 0.1-0.5: 0.05-0.2: 6-30: 1.
in the present invention, preferably, in the step (2), the initiator is one of potassium persulfate, ammonium persulfate and sodium persulfate.
Preferably, in the step (2), the weight ratio of the initiator solution to the glycerol trimethylolpropane triacrylate is 0.5-2: 1; the mass concentration of the initiator solution is 5-10%.
Preferably, in step (2), the reducing agent is sodium sulfite or sodium thiosulfate.
Preferably, in the step (2), the weight ratio of the reducing agent solution to the glycerol trimethylolpropane triacrylate is 0.5-2: 1; the mass concentration of the reducing agent solution is 3-5%.
In the present invention, preferably, in step (3), the temperature of the melt spinning in the melt spinning is 200-250 ℃, the multiple of the drawing is 3-6 times, the temperature of the drawing is 70-100 ℃, and the winding speed is 500-1000 m/min.
The invention also discloses a temporary plugging agent prepared by the method, wherein the molecular structural formula of the temporary plugging agent is as follows:
wherein:
a=50-1000
b=50-500
c=50-500
d=20-500
e=20-200
f=50-1000
g=50-500
h=50-500
i=20-500
j=20-200
k=50-1000
l=50-500
m=50-500
n=20-500
o=20-200
x=2-50
the molecular weight of the temporary plugging agent is 400000-4000000.
The reaction equation for the synthesis of the temporary plugging agent of the invention is as follows:
the third purpose of the invention is to disclose the application of the temporary plugging agent prepared by the method in low permeability reservoir fracturing.
The temporary plugging agent is an aqueous phase five-membered high polymer which takes 2- (allyl dimethyl silyl) pyridine, 1-vinyl-2-pyrrolidone, allyl alcohol polyoxyethylene ether and allyl trimethyl ammonium chloride as polymer raw materials and glycerol trihydroxypropyl ether triacrylate as a cross-linking agent. The polyoxyethylene ether, allyl alcohol, acrylic acid and other groups have good water absorption, and the volume of the product can be greatly improved after water absorption, so that the blocking swept volume is improved; pyridine and pyrrolidone can improve the rigid structure of the molecules and improve the shear resistance of the temporary plugging agent; quaternary ammonium salt, pyridine and polyoxyethylene ether are good surfactants, are beneficial to infiltrating a hydrophobic section of a stratum to improve the blocking rate, and silane reacts with hydroxyl on the surface of the stratum sandstone to increase the lipophilicity of rock, increase the flow resistance of water and improve the blocking rate; span 60 and sodium dodecyl sulfate are typical nonionic surfactants, so that the polymerization quality and uniformity can be improved, the molecular weight of a polymer is increased, the hydrophobic section of a infiltrated stratum is favorably improved, the blocking rate is favorably improved, and the flowback after temporary blocking construction is favorably realized; the glycerol trimethylolpropane ether triacrylate as cross-linking agent can change the one-dimensional linear structure of whole molecule into two-or three-dimensional network structure, and the external layer of whole molecule is hydrophobic, so increasing the flow resistance of water and blocking power. Meanwhile, the temporary plugging agent has a unique appearance structure, the plugging effective rate is greatly improved, no damage is caused to a production layer, the fracturing transformation effect is improved, and the yield after fracturing measures is greatly improved.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts six steps of synthesis, melting, spinning, weaving, cutting and drying to directly obtain the finished product, the preparation method is simple and easy to operate, and the general civil spinning and weaving equipment can be used for industrial production and is beneficial to industrial production;
(2) the temporary plugging agent is synthesized by a one-pot method, the raw materials are easy to obtain, the synthesis process is simple, and no by-product is generated;
(3) the degradation time of the temporary plugging agent can be controlled to be 12-48h by adjusting the formula of the raw materials; meanwhile, the blocking rate and the unblocking rate are high and can reach more than 98 percent, so that the fracturing construction requirement is met;
(4) the temporary plugging agent can completely plug fractured perforation holes, the pressure difference bearing strength of a low-permeability reservoir exceeds 100MPa, an expensive setting tool is not required to be put in before plugging, and only the simplest pumping fluid is required to be added into the temporary plugging agent.
Drawings
FIG. 1 shows a temporary plugging agent M of the present invention 2 Schematic appearance diagram of (1);
FIG. 2 shows a temporary plugging agent M of the present invention 2 Is infrared ray ofA spectrogram.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Example 1
(1) Purging the reactor for 2min with nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 5mol of 2- (allyldimethylsilyl) pyridine, 3mol of 1-vinyl-2-pyrrolidone, 1mol of allyl alcohol polyoxyethylene ether, 0.2mol of allyltrimethylammonium chloride, 42.8g of span 60, 21.4g of sodium dodecyl sulfate and 6500g of water, ensuring slight positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH with 10wt% of sodium hydroxide solution to 6-7;
(2) heating the emulsion to 40 ℃, slowly dropwise adding 214g of 5wt% ammonium persulfate solution into an overhead tank, simultaneously dropwise adding 500g of 3.2wt% sodium sulfite solution, heating to 60 ℃ in the dropwise adding process, continuously stirring for 2 hours after dropwise adding is finished, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 200 ℃, the drafting multiple is 3 times, the drafting temperature is 70 ℃, and the winding speed is 500 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the thread end of the temporary plugging agent into the temporary plugging agentA rope; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 1 。
Example 2
(1) Purging the reactor for 2min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 1mol of 2- (allyl dimethyl silyl) pyridine, 3mol of 1-vinyl-2-pyrrolidone, 0.2mol of allyl alcohol polyoxyethylene ether, 1mol of allyl trimethyl ammonium chloride, 180g of span 60, 85.6g of sodium dodecyl sulfate and 5000g of water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 40 ℃, slowly dropwise adding 956g of 8wt% ammonium persulfate solution into an elevated tank, and simultaneously dropwise adding 214g of 4.2wt% sodium sulfite solution, wherein in the dropwise adding process, the reaction releases heat, the temperature is automatically increased, and simultaneously, after the dropwise adding is finished, heating to 65 ℃, continuously stirring for 2 hours, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 205 ℃, the drawing multiple is 3 times, the drawing temperature is 75 ℃, and the winding speed is 550 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 3 。
Example 3
(1) Purging the reactor for 3min with nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 2mol of 2- (allyldimethylsilyl) pyridine, 0.7 mol of 1-vinyl-2-pyrrolidone, 4mol of allyl alcohol polyoxyethylene ether, 1.2 mol of allyl trimethyl ammonium chloride, 150g of span 60, 38g of sodium dodecyl sulfate and 2568 g of water, ensuring slight positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 42 ℃, slowly dropwise adding 519g of 6wt% ammonium persulfate solution into the elevated tank, and dropwise adding 956g of 3.5wt% sodium sulfite solution, wherein in the dropwise adding process, the reaction releases heat, the temperature is automatically increased, and after the dropwise adding is finished, heating to 62 ℃, continuously stirring for 3 hours, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 220 ℃, the drafting multiple is 4 times, the drafting temperature is 80 ℃, and the winding speed is 600 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the temporary plugging agent thread ends into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 3 。
Example 4
(1) Purging the reactor for 3min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 0.5mol of 2- (allyl dimethyl silyl) pyridine, 1mol of 1-vinyl-2-pyrrolidone, 1mol of allyl alcohol polyoxyethylene ether, 0.9 mol of allyl trimethyl ammonium chloride, 110g of span 60, 39g of sodium dodecyl sulfate and 12840g of water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 45 ℃, slowly dropwise adding 480g of 7wt% sodium persulfate solution into a head tank, simultaneously dropwise adding 480g of 4.5wt% sodium sulfite solution, heating to 63 ℃ in the dropwise adding process, continuously stirring for 3 hours after the dropwise adding is finished, and reacting to form high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 225 ℃, the drafting multiple is 4 times, the drafting temperature is 90 ℃, and the winding speed is 800 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 4 。
Example 5
(1) Purging the reactor for 2min with nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 4mol of 2- (allyldimethylsilyl) pyridine, 3mol of 1-vinyl-2-pyrrolidone, 4mol of allyl alcohol polyoxyethylene ether, 0.6mol of allyltrimethylammonium chloride, 125g of span 60, 74g of sodium dodecyl sulfate and 7000g of water, ensuring a slight positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 with 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 45 ℃, slowly dropwise adding 580g of 10wt% sodium persulfate solution into an overhead tank, simultaneously dropwise adding 580g of 4wt% sodium sulfite solution, heating to 62 ℃ in the dropwise adding process, continuously stirring for 3 hours after the dropwise adding is finished, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 230 ℃, the drawing multiple is 4 times, the drawing temperature is 95 ℃, and the winding speed is 750 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent thread end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 5 。
Example 6
(1) Purging the reactor for 3min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 4mol of 2- (allyl dimethyl silyl) pyridine, 5mol of 1-vinyl-2-pyrrolidone, 3mol of allyl alcohol polyoxyethylene ether, 1.5mol of allyl trimethyl ammonium chloride, 89g of span 60, 55g of sodium dodecyl sulfate and 6000g of water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 43 ℃, slowly dropwise adding 426g of 7wt% sodium persulfate solution into the elevated tank, and simultaneously dropwise adding 426g of 3wt% sodium thiosulfate solution, wherein in the dropwise adding process, the reaction releases heat, the temperature is automatically increased, and simultaneously, after the dropwise adding is finished, heating to 60 ℃, continuously stirring for 2 hours, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 245 ℃, the drafting multiple is 5 times, the drafting temperature is 85 ℃, and the winding speed is 900 m/min.
(4) By means of braiding machinesWeaving the temporary plugging agent composite thread produced in the step (3) to manufacture a temporary plugging agent thread end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 6 。
Example 7
(1) Purging the reactor for 2min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 0.5mol of 2- (allyldimethylsilyl) pyridine, 0.5mol of 1-vinyl-2-pyrrolidone, 0.2mol of allyl alcohol polyoxyethylene ether, 0.2mol of allyl trimethyl ammonium chloride, 120g of span 60, 60g of sodium dodecyl sulfate and 7200g of water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 41 ℃, slowly dropwise adding 600g of 6wt% potassium persulfate solution into the elevated tank, simultaneously dropwise adding 600g of 5wt% sodium thiosulfate solution, heating to 65 ℃ in the dropwise adding process, continuously stirring for 2.5 hours after the dropwise adding is finished, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 240 ℃, the drawing multiple is 5 times, the drawing temperature is 90 ℃, and the winding speed is 920 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent thread end with uniform thickness; then weaving the temporary plugging agent thread ends into temporary plugging agent ropes; then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, drying and preparing the degradable rope knot type temporary plugging agent M for fracturing 7 。
Example 8
(1) Purging the reactor for 3min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane triacrylate, 4mol of 2- (allyl dimethyl silyl) pyridine, 4mol of 1-vinyl-2-pyrrolidone, 5mol of allyl alcohol polyoxyethylene ether, 2mol of allyl trimethyl ammonium chloride, 180g of span 60, 80g of sodium dodecyl sulfate and 6200g of water, ensuring slight positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 44 ℃, slowly dripping 440g of 9wt% potassium persulfate solution into the elevated tank, dripping 440g of 4wt% sodium thiosulfate solution into the elevated tank, wherein in the dripping process, the reaction releases heat, the temperature is automatically increased, and after the dripping is finished, heating to 65 ℃, continuously stirring for 2.5 hours, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of the melt spinning in the melt spinning is 245 ℃, the drafting multiple is 4 times, the drafting temperature is 95 ℃, and the winding speed is 850 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the temporary plugging agent thread ends into temporary plugging agent ropes; then the temporary plugging agent rope is knotted and the rope ends at the two ends of the rope knot are scattered, and the degradable rope knot type temporary plugging agent M for fracturing is prepared after drying 8 。
Example 9
(1) Purging the reactor for 2min by nitrogen, sequentially adding 1mol of glycerol trimethylolpropane ether triacrylate, 5mol of 2- (allyl dimethyl silyl) pyridine, 5mol of 1-vinyl-2-pyrrolidone, 5mol of allyl alcohol polyoxyethylene ether, 2mol of allyl trimethyl ammonium chloride, 214g of span 60, 24g of sodium dodecyl sulfate and 3600g of water, ensuring a slight positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using a 10wt% sodium hydroxide solution;
(2) heating the emulsion to 43 ℃, slowly dropwise adding 240g of 7wt% potassium persulfate solution into an overhead tank, simultaneously dropwise adding 240g of 4wt% sodium thiosulfate solution, heating to 64 ℃ in the dropwise adding process, continuously stirring for 2 hours after the dropwise adding is finished, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
the temperature of melt spinning in the melt spinning is 250 ℃, the drafting multiple is 6 times, the drafting temperature is 100 ℃, and the winding speed is 1000 m/min.
(4) Weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the temporary plugging agent thread ends into temporary plugging agent ropes; then the temporary plugging agent rope is knotted and the rope ends at the two ends of the rope knot are scattered, and the degradable rope knot type temporary plugging agent M for fracturing is prepared after drying 9 。
Test example 1 measurement of expansion factor
80000mg/L of sodium chloride solution is added into a series of pressure-resistant wide-mouth bottles respectively, the oil bath is heated to 90 ℃, the temporary plugging agent is added, the oil bath is heated to 90 ℃, the glass bottles are taken out at intervals, the temporary plugging agent in the glass bottles is poured into a standard sieve for filtration, the filtered water is put back into the wide-mouth bottles, the mass of the temporary plugging agent is rapidly weighed, the temporary plugging agent is put back into the wide-mouth bottles, the temperature is kept constant for 90 ℃, the expansion multiple n is calculated, and the test results are shown in table 1.
n=m 1 /m 0
In the formula: n: expansion times;
m 1 : mass, g, of the temporary plugging agent after expansion;
m 0 : mass of temporary plugging agent, g.
TABLE 1 test results of expansion factor at different times
As can be seen from table 1: temporary plugging agent M 1 -M 9 The expansion times at different times are different, and the expansion times are increased along with the extension of time, the expansion times are more than 12 times at 15min, and the expansion times of HJK-7 are 5.7 times; the expansion factor is more than 20 times at 60min, and the expansion factor of HJK-7 is 11.5 times; the expansion factor is more than 23 times at 150min, and the expansion factor of HJK-7 is 13.7 times. The expansion times of the temporary plugging agent HJK-7 are significantly lower than those of the temporary plugging agent of the present invention, and the difference of the expansion times is more significant with the time.
Test example 2 measurement of degradation time
After the test of the test example 1 is continuously performed for 150min, the temporary plugging agent basically does not absorb water any more, the temporary plugging agent is continuously placed in a wide-mouth bottle, after a period of time, the temporary plugging agent is gradually dissolved, the time after the temporary plugging agent is completely dissolved is the degradation time of the temporary plugging agent, and the test results are shown in table 2.
TABLE 2 test results of degradation time, surface tension, temporary plugging rate, and permeability recovery
As can be seen from Table 2, there is a significant difference in the degradation time of the temporary plugging agent, with the longest M being 9 48h, shortest M 7 Is 12 h. The more the amount of glycerol trimethylolpropane triacrylate is added, the easier it is to dissolve and the shorter the degradation time, and vice versa.
Therefore, the degradation time can be determined according to the construction operation requirement during field application, so that the proportion of the monomer glycerol trimethylolpropane triacrylate of the blocking remover can be selected, and the degradation time of the temporary blocking remover can be controlled between 12 and 48 hours.
Test example 3 measurement of surface tension
After the samples in test example 2 were completely degraded, the surface tension of the solution was measured by a ring pulling method, and the results are shown in Table 2.
As can be seen from table 2: temporary plugging agent M 1 -M 9 The surface tension is less than 27mN/m, the surface tension of HJK-7 is 36.8mN/m, and the surface tension of the temporary plugging agent is obviously lower than that of the temporary plugging agent sold in the market HJK-7.
Test example 4 determination of temporary plugging Rate and Permeability recovery Rate
The temporary plugging rate and the permeability recovery rate are tested by referring to Q/SH 10202187-2018 Universal technical Condition of Water-soluble temporary plugging agent, and the test results are shown in Table 2.
As can be seen from table 2: temporary plugging agent M 1 -M 9 The temporary plugging rate is more than 99 percent, wherein M 2 The temporary plugging rate reaches 99.8 percent to the maximum, and the temporary plugging rate of HJK-7 is 85.2 percent; temporary plugging agent M 1 -M 9 The recovery rates of (A) and (B) are all more than 98%, wherein M is 9 The recovery rate of the product reaches 98.7 percent at most, while the recovery rate of HJK-7 is 90.2 percent. The temporary plugging rate and recovery rate of the temporary plugging agent are obviously higher than those of the temporary plugging agent HJK-7. The temporary plugging agent has good temporary plugging and unblocking effects.
Test example 5 test of blocking Strength
At 90 ℃, manually manufacturing a sealing rock core by adopting different permeability rates, squeezing and injecting 1PV 10g/L of temporary plugging agent concentration, and testing the sealing strength of the sealing agent, wherein the test results are shown in table 3.
Table 3 core plugging strength test results with different permeabilities
As can be seen from table 3:
(1) for low permeability cores, temporary plugging agent M 1 -M 9 The plugging strength of (A) is more than 100MPa, wherein M 8 The highest reaches 129.2MPa, and the plugging strength of HJK-7 is 4.5MPa, which is obviously lower than that of the invention;
(2) for high permeability core, temporary plugging agent M 1 -M 9 The plugging strength of (A) is more than 70MPa, wherein M 4 The highest reaches 79.8MPa, and the plugging strength of HJK-7 is 4.0MPa, which is obviously lower than that of the invention.
Experimental example 6 Infrared Spectroscopy characterization
Product M by infrared spectroscopy 2 The characterization was performed and the results are shown in fig. 1.
As can be seen from FIG. 1, 2922cm -1 Is abundantly present in the molecule
A key expansion vibration absorption peak; 1732cm -1 Formed from pyrrolidones
A key expansion vibration absorption peak; 1233cm -1 Is polyoxyethylene ether
A key expansion vibration absorption peak; 1163cm -1 Formed from acrylic esters
A bond strength absorption characteristic peak; 1012cm -1 、656cm -1 Is in quaternary ammonium salt
Key stretching vibration and bending vibration absorption peaks.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (9)
1. A preparation method of a degradable rope knot type temporary plugging agent for fracturing comprises the following steps:
(1) purging the reactor for 2-3min by nitrogen, sequentially adding glycerol trimethylolpropane triacrylate, 2- (allyl dimethyl silyl) pyridine, 1-vinyl-2-pyrrolidone, allyl alcohol polyoxyethylene ether, allyl trimethyl ammonium chloride, span 60, sodium dodecyl sulfate and water, ensuring micro-positive pressure by nitrogen, starting stirring until all raw materials are completely uniform emulsion, and adjusting the pH to 6-7 by using 10wt% of sodium hydroxide solution;
(2) heating the emulsion to 40-45 ℃, slowly dripping an initiator solution into the elevated tank, dripping a reducing agent solution into the elevated tank, wherein in the dripping process, the reaction releases heat, the temperature is automatically increased, and after finishing dripping, heating to 60-65 ℃, continuously stirring for 2-3h, and reacting to form a high-viscosity polymer solution; granulating the polymerization solution to obtain a temporary plugging agent with the particle diameter of 0.1-1 mm;
(3) drying the temporary plugging agent, then carrying out melt spinning, cooling, oiling, drafting and winding to obtain temporary plugging agent spinning; secondly, spinning the temporary plugging agent by using a spinning machine to generate a temporary plugging agent composite thread;
(4) weaving the temporary plugging agent composite wire produced in the step (3) by using a weaving machine to manufacture a temporary plugging agent wire end with uniform thickness; then weaving the thread ends of the temporary plugging agent into temporary plugging agent ropes; and then knotting the temporary plugging agent rope, scattering rope ends at two ends of the rope knots, and drying to prepare the degradable rope knot type temporary plugging agent for fracturing.
2. The method according to claim 1, wherein the 2- (allyldimethylsilyl) pyridine, the 1-vinyl-2-pyrrolidone, the allyloxyethyleneether, and the allyltrimethylammonium chloride are used in an amount of 0.5 to 5 parts by mole, 0.2 to 5 parts by mole, and 0.2 to 2 parts by mole, respectively, based on 1 part by mole of the glycerol trimethylolpropane triacrylate.
3. The method according to claim 1, wherein in the step (1), the weight ratio of span 60, sodium lauryl sulfate, water and glycerol trimethylolpropane triacrylate is 0.1-0.5: 0.05-0.2: 6-30: 1.
4. the method according to claim 1, wherein in the step (2), the initiator is one of potassium persulfate, ammonium persulfate and sodium persulfate.
5. The method according to claim 1, wherein the weight ratio of the initiator solution to the glycerol trimethylolpropane triacrylate is 0.5-2: 1; the mass concentration of the initiator solution is 5-10%.
6. The method according to claim 1, wherein in the step (2), the reducing agent is sodium sulfite or sodium thiosulfate.
7. The method according to claim 1, wherein the weight ratio of the reducing agent solution to the glycerol trimethylolpropane triacrylate is in the range of 0.5 to 2: 1; the mass concentration of the reducing agent solution is 3-5%.
8. The preparation method according to claim 1, wherein in the step (3), the temperature of the melt spinning in the melt spinning is 200-250 ℃, the drawing multiple is 3-6 times, the drawing temperature is 70-100 ℃, and the winding speed is 500-1000 m/min.
9. The degradable knot type temporary plugging agent for fracturing prepared by the preparation method according to any one of claims 1 to 8, wherein the molecular structural formula of the temporary plugging agent is as follows:
wherein:
a=50-1000；
b=50-500；
c=50-500；
d=20-500；
e=20-200；
f=50-1000；
g=50-500；
h=50-500；
i=20-500；
j=20-200；
k=50-1000；
l=50-500；
m=50-500；
n=20-500；
o=20-200；
x=2-50；
the molecular weight of the temporary plugging agent is 400000-4000000.
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| CN107287674A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of soluble fine-denier PVA fibers and application thereof |
| CN108300439A (en) * | 2017-12-13 | 2018-07-20 | 北京捷贝通石油技术有限公司 | A kind of temporary stall of well fracturing is to water-soluble diverting agent and preparation method thereof |
| CN110344132A (en) * | 2019-07-29 | 2019-10-18 | 西安工程大学 | A kind of preparation method of temperature control pressure break temporarily stifled fiber |
| CN111334886A (en) * | 2020-04-16 | 2020-06-26 | 陕西科技大学 | Temporary plugging agent for oil well prepared from covalent bond crosslinked polyvinyl alcohol landfill initiator and preparation method thereof |
| CN111484578A (en) * | 2020-04-23 | 2020-08-04 | 四川轻化工大学 | Water-soluble AA-AM-NVP-NGD quadripolymer temporary plugging agent for fracturing and synthesis method thereof |
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Patent Citations (5)
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| CN107287674A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工集团公司 | A kind of soluble fine-denier PVA fibers and application thereof |
| CN108300439A (en) * | 2017-12-13 | 2018-07-20 | 北京捷贝通石油技术有限公司 | A kind of temporary stall of well fracturing is to water-soluble diverting agent and preparation method thereof |
| CN110344132A (en) * | 2019-07-29 | 2019-10-18 | 西安工程大学 | A kind of preparation method of temperature control pressure break temporarily stifled fiber |
| CN111334886A (en) * | 2020-04-16 | 2020-06-26 | 陕西科技大学 | Temporary plugging agent for oil well prepared from covalent bond crosslinked polyvinyl alcohol landfill initiator and preparation method thereof |
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