CN106833598A - Degradable fracturing propping agent and preparation method thereof - Google Patents
Degradable fracturing propping agent and preparation method thereof Download PDFInfo
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- CN106833598A CN106833598A CN201611085065.6A CN201611085065A CN106833598A CN 106833598 A CN106833598 A CN 106833598A CN 201611085065 A CN201611085065 A CN 201611085065A CN 106833598 A CN106833598 A CN 106833598A
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- fracturing propping
- propping agents
- degradable
- degradable fracturing
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 57
- 229920001577 copolymer Polymers 0.000 claims abstract description 15
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000881 Modified starch Polymers 0.000 claims abstract description 13
- 239000004368 Modified starch Substances 0.000 claims abstract description 13
- 235000019426 modified starch Nutrition 0.000 claims abstract description 13
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 7
- 239000004310 lactic acid Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 11
- 229920002261 Corn starch Polymers 0.000 claims description 10
- 239000008120 corn starch Substances 0.000 claims description 10
- 229940099112 cornstarch Drugs 0.000 claims description 10
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 10
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 10
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 229910019213 POCl3 Inorganic materials 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N Vilsmeier-Haack reagent Natural products CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- -1 Dimethylformamide dimethyl acid amides Chemical class 0.000 claims description 2
- 238000003808 methanol extraction Methods 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 2
- 239000010779 crude oil Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 2
- 239000003921 oil Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229920000578 graft copolymer Polymers 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- AIDQCFHFXWPAFG-UHFFFAOYSA-N n-formylformamide Chemical compound O=CNC=O AIDQCFHFXWPAFG-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/80—Compositions for reinforcing fractures, e.g. compositions of proppants used to keep the fractures open
- C09K8/805—Coated proppants
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/06—Esters of inorganic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a degradable fracturing propping agent and a preparation method thereof. The degradable fracturing propping agent comprises inorganic salt and a copolymer wrapping the inorganic salt; the copolymer is obtained by graft copolymerization of modified starch and lactic acid under the action of a catalyst. The invention also provides a preparation method of the degradable fracturing propping agent, and the degradable fracturing propping agent provided by the invention has the advantages of low cost and simple preparation process, and can effectively improve the recovery ratio of crude oil.
Description
Technical field
The present invention relates to a kind of fracturing propping agents and preparation method thereof, more particularly to a kind of degradable fracturing propping agents and
Its preparation method, belongs to technical field of petrochemical industry.
Background technology
Fracturing Technology plays very important effect to oil exploitation, and fracturing propping agents (a kind of ceramic particle is produced
Product, with fracturing strengh very high, are mainly used in oil field well support, to increase the yield of petroleum gas) it is oil fracturing
The key that can technology succeed.
During fine and close oil gas, the pressure break such as hypotonic, Oil in Super-low Permeability oil field, the crack for wanting to form pressure break does not close, stone
Oily product is unimpeded to be flowed through, and can enter stratum together with fracturing fluid by proppant, fills the crack of rock stratum, the release of stress
Closure would not be caused, in order to improve Oil Guide rate, increases crude output.The research of degradable proppant is opened more to Middle-Low Permeability Reservoirs
Big drain path, obtains production capacity higher significant.
At present, have to low-density, in high-strength sintered haydite research, the hollow or porous propping agent development of low-density,
Double-layer resin coating technology research, but the research to degradable fracturing propping agents is not yet reported.
The content of the invention
In order to solve the above-mentioned technical problem, it is an object of the invention to provide a kind of degradable proppant, the proppant rises
To after isolation supporting role, bigger drain path is opened in a part of degradable proppant degraded, is improved fracture condudtiviy and is increased
Plus the recovery ratio of crude oil.
In order to realize above-mentioned technical purpose, the invention provides a kind of degradable fracturing propping agents, the degradable pressure break branch
Support agent includes the copolymer of inorganic salts and parcel inorganic salts；Wherein, copolymer is made in catalyst by modified starch and lactic acid
Under, obtained by graft copolymerization.
Graft copolymerization refers to that the polymer different from backbone chemistry structure are connected on some atoms of main polymer chain
A kind of copolymer of the side chain of segment, referred to as graft copolymer, such as graft chloroprene rubber, SBS graft copolymers.
In the degradable fracturing propping agents that the present invention is provided, it is preferable that the inorganic salts for using are potassium chloride.
In the degradable fracturing propping agents that the present invention is provided, it is preferable that the modified starch of use is led to by cornstarch
Cross and be modified what is obtained.
In the degradable fracturing propping agents that the present invention is provided, it is preferable that Malaysia is used when being modified to cornstarch
Acid anhydrides, sodium metaperiodate, POCl3 are modifying agent；It is highly preferred that the mixing quality of maleic anhydride, sodium metaperiodate, POCl3
Than being 5:4:3.
In the degradable fracturing propping agents that the present invention is provided, it is preferable that diformazan is used when being modified to cornstarch
Base diformamide is solvent.
In the degradable fracturing propping agents that the present invention is provided, it is preferable that the catalyst includes that zinc chloride and octanoic acid are sub-
Tin, wherein, the mass ratio of zinc chloride and stannous octoate is 4:3.
Present invention also offers the preparation method of above-mentioned degradable fracturing propping agents, the preparation method is comprised the following steps：
Modified starch and lactic acid is gelatinized under 75 DEG C -85 DEG C (preferably 80 DEG C) (preferably 1.5 was small in -2 hours 1 hour
When)；
Dehydration to bubble-free dry-steam outflow is vacuumized under 100 DEG C -110 DEG C (preferably 105 DEG C), catalyst is added
It is warming up to 120 DEG C -135 DEG C (preferably 130 DEG C) and reacts -6 hours 5 hours (preferably 5 hours), is warming up to 140 DEG C -145 DEG C
(preferably 140 DEG C) react -16 hours 14 hours (15 hours)；
Product obtains copolymer by dissolving, precipitation, centrifugation, drying；
Inorganic salts are wrapped up using copolymer, obtains degradable fracturing propping agents.
In the preparation method of the degradable fracturing propping agents that the present invention is provided, it is preferable that modified starch is by following step
Suddenly prepare：
Cornstarch is improved in containing modifying agent, the aqueous solution of solvent, wherein, the quality of modifying agent and solvent
Mixing ratio is 0.35：2.3, product is dried under 70 DEG C -75 DEG C (preferably 70 DEG C), obtains modified starch.
In the preparation method of the degradable fracturing propping agents that the present invention is provided, it is preferable that using chloroform dissolving.
In the preparation method of the degradable fracturing propping agents that the present invention is provided, it is preferable that use methanol extraction.
Specific embodiment of the invention, when copolymer is wrapped up inorganic salts by the way of this area is general
, wrapped up using the such as industrial packing machine of processing machine in the present invention.
In the preparation method of degradable fracturing propping agents of the invention, when dehydration is vacuumized, pressure is 0.085MPa
Preferably.
The above-mentioned degradable fracturing propping agents that the present invention is provided, do not have during specifically for construction with the method for general proppant
Have any different, construct in a conventional manner.
The degradable fracturing propping agents that the present invention is provided, stratum is entered with general proppant (haydite or quartz sand) together,
After arrival target zone plays isolation supporting role, bigger drain path is opened in a part of degradable proppant degraded, and raising is split
Seam flow conductivity increases the recovery ratio of crude oil.
The cornstarch of the degradable fracturing propping agents use that the present invention is provided, lactic acid, these material prices of inorganic salts are low
It is honest and clean, advantageously reduce the cost of proppant.
The preparation process is simple of the degradable fracturing propping agents that the present invention is provided.
Specific embodiment
In order to be more clearly understood to technical characteristic of the invention, purpose and beneficial effect, now to skill of the invention
Art scheme carry out it is described further below, but it is not intended that to it is of the invention can practical range restriction.
Embodiment 1
Present embodiments provide a kind of degradable fracturing propping agents, itself through the following steps that prepare：
The preparation of modified starch：At modifying agent (maleic anhydride 0.15g, sodium metaperiodate 0.12g, POCl3 0.08g), fit
Cornstarch 10kg is improved in the aqueous solution of amount shallow lake agent (dimethylformamide dimethyl acid amides 2.30), product is dried standby at 70 DEG C
With；
The preparation of copolymer：After above-mentioned modified starch 8kg and lactic acid 100L is gelatinized 1.5 hours at 80 DEG C, at 105 DEG C
(0.085MPa) dehydration to system bubble-free dry-steam outflow is vacuumized, zinc oxide 0.60g, stannous octoate 0.45g liters is added
130 DEG C of temperature is reacted 5 hours, is heated up 140 DEG C and is reacted 15 hours；Product chloroform is dissolved into (insoluble matter filters removal) heavy with methyl alcohol
Shallow lake, centrifugation, repeatedly by product dissolution precipitation, by the copolymer of drying precipitate；
Copolymer is wrapped up inorganic salts in processing machine, degradable fracturing propping agents are finally given.
Above-mentioned degradable fracturing propping agents manufactured in the present embodiment are carried out with dissolution experiment, the experiment of rock core flow conductivity, with
Test its solubility property, improve stratum flow conductivity performance.
1st, solubility property experiment：
The above-mentioned degradable fracturing propping agents (weight 5g) of the present embodiment are placed in the beaker for filling 250mL water, not equality of temperature
Dissolution time under degree, test result is as shown in table 1.
The solubility property experimental result of the degradable fracturing propping agents of table 1
| 30℃ | 45℃ | 60℃ | 70℃ | 100℃ | |
| Sample | - | - | 6h | 3h | 1h |
2nd, flow conductivity performance test：Test degradable fracturing propping agents guide performance
Above-mentioned degradable fracturing propping agents and quartz sand are added into 1# artificial cores (porosity 12.44%) together, it is identical
The quartz sand of quality is added under 2# artificial cores simulation same formation pressure condition, and being acidified flowing by rock core evaluates instrument (SL32-
180 types), influence of the degradable fracturing propping agents to guide performance is tested, test result is as shown in table 2.
The breakthrough pressure experimental result of the diverting agent of table 2
| Sample name | |
| 1# | 2.378 |
| 2# | 1.867 |
Above example illustrates, the solubility property of degradable fracturing propping agents of the invention is good, to the water conservancy diversion energy on stratum
Power improves, and can effectively improve the recovery ratio of crude oil.
Claims (10)
1. a kind of degradable fracturing propping agents, it is characterised in that the degradable fracturing propping agents include inorganic salts and parcel nothing
The copolymer of machine salt；Wherein, the copolymer is by modified starch and lactic acid under catalyst action, by graft copolymerization
Obtain.
2. degradable fracturing propping agents according to claim 1, it is characterised in that the inorganic salts are potassium chloride.
3. degradable fracturing propping agents according to claim 1, it is characterised in that the modified starch is by cornstarch
By being modified what is obtained.
4. degradable fracturing propping agents according to claim 3, it is characterised in that used when being modified to cornstarch
Maleic anhydride, sodium metaperiodate, POCl3 are used as modifying agent；Preferably, the maleic anhydride, sodium metaperiodate, POCl3
Mixing quality ratio is 5:4:3.
5. degradable fracturing propping agents according to claim 3, it is characterised in that used when being modified to cornstarch
Dimethylformamide dimethyl acid amides is solvent.
6. degradable fracturing propping agents according to claim 1, it is characterised in that the catalyst includes zinc chloride and pungent
Sour stannous, wherein, the mass ratio of zinc chloride and stannous octoate is 4:3.
7. the preparation method of the degradable fracturing propping agents described in any one of claim 1-6, it is characterised in that the preparation method
Comprise the following steps：
Modified starch and lactic acid are gelatinized -2 hours 1 hour at 75 DEG C -85 DEG C；
Dehydration to bubble-free dry-steam outflow is vacuumized at 100 DEG C -110 DEG C, catalyzer temperature-elevating is added to 120 DEG C -135 DEG C
Reaction 5-6 hours, is warming up to 140 DEG C -145 DEG C-reaction 14-16 hours；
Product obtains copolymer by dissolving, precipitation, centrifugation, drying；
Inorganic salts are wrapped up using copolymer, obtains the degradable fracturing propping agents.
8. the preparation method of degradable fracturing propping agents according to claim 7, it is characterised in that modified starch by with
Lower step is prepared：
Cornstarch is improved in containing modifying agent, the aqueous solution of solvent, wherein, the mass mixing of modifying agent and solvent
Than being 0.35：2.3, product is dried at 70 DEG C -75 DEG C, obtains the modified starch.
9. the preparation method of degradable fracturing propping agents according to claim 7, it is characterised in that using chloroform dissolving.
10. the preparation method of degradable fracturing propping agents according to claim 7, it is characterised in that use methanol extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611085065.6A CN106833598A (en) | 2016-12-01 | 2016-12-01 | Degradable fracturing propping agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611085065.6A CN106833598A (en) | 2016-12-01 | 2016-12-01 | Degradable fracturing propping agent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106833598A true CN106833598A (en) | 2017-06-13 |
Family
ID=59145953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611085065.6A Pending CN106833598A (en) | 2016-12-01 | 2016-12-01 | Degradable fracturing propping agent and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN106833598A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110284861A (en) * | 2019-05-20 | 2019-09-27 | 西南石油大学 | A method of intrinsic fracture heavy crude reservoir is exploited using Degradable temporary blocking agent auxiliary SAGD |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110284861A (en) * | 2019-05-20 | 2019-09-27 | 西南石油大学 | A method of intrinsic fracture heavy crude reservoir is exploited using Degradable temporary blocking agent auxiliary SAGD |
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