CN109880609A - A kind of self-crosslinking height takes sand cleaning slippery water and preparation method thereof - Google Patents
A kind of self-crosslinking height takes sand cleaning slippery water and preparation method thereof Download PDFInfo
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- CN109880609A CN109880609A CN201910258636.9A CN201910258636A CN109880609A CN 109880609 A CN109880609 A CN 109880609A CN 201910258636 A CN201910258636 A CN 201910258636A CN 109880609 A CN109880609 A CN 109880609A
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Abstract
The invention discloses a kind of self-crosslinking height to take sand cleaning slippery water, and slippery water is to be added to the water drag reducer to configure；Drag reducer is to carry out polymer emulsion made of biphasic emulsion polymerization reaction under initiator effect interior phase solution and external solution；External solution includes component polyester, green solvent and crosslinking agent；Interior phase solution includes component 2- acrylamide-2-methylpro panesulfonic acid, organic amine and water.Preparation step: (1) polyester, green solvent and crosslinking agent are mixed, obtains external solution；(2) water, 2- acrylamide-2-methylpro panesulfonic acid and organic amine are mixed, obtains interior phase solution；(3) external solution is placed in 30~40 DEG C of water-bath, interior phase solution is added, after leading to nitrogen deoxygenation, initiator is added, seal reactor, 80 DEG C of 4~5h of isothermal reaction obtain self-crosslinking height and take sand cleaning slippery water.Slippery water of the invention gathers multi -function in integral whole, and not only instant and efficient drag reduction has both sterilization, the row of helping and clay stabilization synergistic function.
Description
Technical field
The present invention relates to oil gas field yield-increasing technology fields, and in particular to a kind of self-crosslinking height takes sand cleaning slippery water and its system
Preparation Method.
Background technique
Hydraulic fracturing is always most effective well stimulation technology in oil-gas reservoir recovery process, conventional oil gas well reservoir reconstruction
Gelled fracturing fluid is used, and shale gas well reservoir reconstruction need to use special fracturing fluid, i.e. slippery water fracturing fluid.It is by macromolecule
Or drag reducer, water, the auxiliary agent of Superhigh Molecular Polymer are formulated, and make it have the performance of low viscosity, low frictional resistance, thus substantially
Cost of winning is reduced, very high production capacity is obtained.Therefore, slippery water drag reducer is widely used, and demand is very huge.So
And at present slippery water fracturing fluid drag reducer there is a series of problems, for example, slippery water fracturing fluid need to add fungicide,
The multiple additives such as expansion-resisting agent, cleanup additive, scene is complicated using program, inconvenient, higher cost.
Summary of the invention
It is a variety of the purpose of the present invention is needing to add drag reducer, expansion-resisting agent, cleanup additive etc. for conventional slippery water fracturing fluid
Medicament, and the technological deficiencies such as sand carrying effect difference provide a kind of novel self-crosslinking height and take sand cleaning slippery water.
Self-crosslinking height provided by the invention is taken sand cleaning slippery water and is configured by drag reducer and water, directly adds drag reducer
Enter in water, self-crosslinking reaction is generated in whipping process, forms certain highly viscous slippery water fracturing fluid.The drag reducer be by
It is 500-1000 ten thousand that interior phase solution and external solution carry out molecular weight made of biphasic emulsion polymerization reaction under initiator effect
Polymer emulsion.External solution includes component polyester, green solvent and crosslinking agent；Green solvent is that propylene glycol esters are molten
Agent；Interior phase solution includes component 2- acrylamide-2-methylpro panesulfonic acid, organic amine and water.
The mass percent for preparing the raw material components of drag reducer is as follows: polyester 10-15%, green solvent 10-20%, crosslinking
Agent 1-2%, water 30-45%, 2- acrylamide-2-methylpro panesulfonic acid 10-20%, organic amine 4-8%, initiator 0.01-
0.05%.
Wherein, the polyester is one of polyglycolide, polylactide, glycolide-lactide copolymer, polycaprolactone
Or two kinds of mixture.
The green solvent is propylene glycol methyl ether acetate, in propylene-glycol ethyl ether acetate, propylene glycol butyl ether acetate
A kind of or at least two kinds of mixture.
The crosslinking agent is the double isopropyl zirconates of double triethanolamines, in the double isopropyl zirconic acid ammoniums of dilactic acid, zirconium lactate
It is a kind of.
The organic amine is triethylamine, diethyl propylamine, diethyl butylamine, diethylhexylamine, diethyl octylame or two
One of ethyl decyl amine or at least two mixture.
The initiator is one of azo, over cure acids or peroxy type free radical initiator.
Above-mentioned self-crosslinking height takes the preparation method of sand cleaning slippery water, includes the following steps:
Step 1 is weighed each raw material component for preparing drag reducer: polyester 10-15%, green solvent by following mass percent
10-20%, crosslinking agent 1-2%, water 30-45%, 2- acrylamide-2-methylpro panesulfonic acid 10-20%, organic amine 4-8%, draw
Send out agent 0.01-0.05%.
Step 2 prepares external solution: polyester, green solvent and crosslinking agent being mixed in proportion, stirred evenly, is obtained outer
Phase solution；
Step 3 prepares interior phase solution: water, 2- acrylamide-2-methylpro panesulfonic acid and organic amine mixed in proportion,
And stir evenly, interior phase solution is obtained, it is spare；
Step 4, biphasic emulsion polymerization: external solution is poured into reaction vessel, reaction vessel is placed in 30~40 DEG C
In water bath with thermostatic control, then interior phase solution is slowly added into external solution by turn on agitator, is uniformly mixed, and nitrogen high speed is led to
Deoxygenation is stirred, after stirring 20~40min, initiator is instilled in reaction vessel, it is anti-to be warming up to 80 DEG C of constant temperature for sealed reaction vessel
4~5h is answered, it is cooling, obtain drag reducer；
Drag reducer is added to the water by step 5, stirring, obtains self-crosslinking height and takes sand cleaning slippery water.
Compared with prior art, the invention has the following advantages:
(1) slippery water integrates drop and hinders, sterilizes, preventing the multiple functions such as the swollen, row of helping, and solves conventional slippery water needs
Add drag reducer, fungicide, expansion-resisting agent, the various medicaments such as cleanup additive and caused by scene match liquid complicated for operation, heavy workload, at
This high problem.(2) mineral oil is free of in the system, no biotoxicity is synthesized, wiper ring using nontoxic chemical substance
It protects.It is good from flowback effect, to reservoir permeability without any injury.(3) field application shows that self-crosslinking height takes sand cleaning slippery water
With viscosity higher, sand carrying effect is good, and sand ratio can effectively reduce frictional resistance up to 30%, and solid-carrying performance is excellent, prevents the swollen and row of helping effect
Fruit is good, and low to water quality requirement, and returning drain can reuse, and drag reducing efficiency and other effects remains unchanged, it can be achieved that the row of returning
Water zero discharge improves water blanket utilization rate.(4) heat-resisting quantity is good, and high temperature can be more than 180 DEG C.(5) scene is simple with liquid,
It is easy to use, it can be widely applied in a plurality of types of pressing crack constructions.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
The drag reducer resistance-reducing yield test chart of Fig. 1, embodiment 1.
The 13rd section of construction curve figure of Fig. 2, XX03 well.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1
For preparing 200 grams of drag reducers, which takes sand cleaning slippery water for configuring self-crosslinking height.
Drag reducer is prepared, steps are as follows:
Step 1 prepares external solution: 30 grams of polylactides, 30 grams of propylene-glycol ethyl ether acetates and 4 grams of zirconium lactates are carried out
Mixing, stirs evenly, obtains external solution；
Step 2 prepares interior phase solution: by 80 grams of water, 40 grams of 2- acrylamide-2-methylpro panesulfonic acids and 14 grams of diethyl
Butylamine mixing, and stir evenly, interior phase solution is obtained, it is spare；
External solution is poured into 250mL three-necked flask by step 3, and three-necked flask is placed in 30 DEG C of constant temperature water bath,
It is stirred continuously；Interior phase solution is slowly dropped into external solution again, so that it is filled mixing, is made into base fluid, leads to nitrogen high-speed stirred
Deoxygenation after stirring 20~40min, 2 milliliters of 5% ammonium persulfate aqueous solution is slowly added dropwise in reaction vessel be catalyzed and is drawn
Hair, sealed reaction vessel are warming up to 80 DEG C of isothermal reaction 4h, cooling, obtain polymer drag reducer.
The polymer drag reducer is added to the water, stirring, obtains self-crosslinking height and takes sand cleaning slippery water.
Embodiment 2
Above-mentioned self-crosslinking height takes the preparation method of sand cleaning slippery water, includes the following steps:
Step 1, prepare external solution: by 150 grams of glycolide-lactide copolymers, 100 grams of propylene glycol methyl ether acetates and
19.5 grams of double double isopropyl zirconates of triethanolamine are mixed, and are stirred evenly, are obtained external solution；
Step 2 prepares interior phase solution: by 300 grams of water, 100 grams of 2- acrylamide-2-methylpro panesulfonic acids and 40 gram of three second
Amine mixing, and stir evenly, interior phase solution is obtained, it is spare；
External solution is poured into reaction vessel by step 3, and reaction vessel is placed in 40 DEG C of constant temperature water bath, constantly
Stirring；Interior phase solution is slowly dropped into external solution again, so that it is filled mixing, is made into base fluid, leads to the deoxygenation of nitrogen high-speed stirred,
After stirring 40min, 0.5 gram of two NSC 18620 salt of azo is dissolved in a small amount of water, it is then that two NSC 18620 saline solution of azo is slow
It being added dropwise in reaction vessel and carries out catalysis initiation, sealed reaction vessel is warming up to 80 DEG C of isothermal reaction 5h, and it is cooling, it is polymerize
Object drag reducer.
Drag reducer is added to the water by step 4, stirring, obtains self-crosslinking height and takes sand cleaning slippery water.
Embodiment 3
Above-mentioned self-crosslinking height takes the preparation method of sand cleaning slippery water, includes the following steps:
Step 1 prepares external solution: by the double creams of 100 grams of polycaprolactones, 150 grams of propylene glycol butyl ether acetates and 19.5 grams
Sour double isopropyl zirconic acid ammoniums are mixed, and are stirred evenly, are obtained external solution；
Step 2 prepares interior phase solution: by 450 grams of water, 200 grams of 2- acrylamide-2-methylpro panesulfonic acids and 80 grams of diethyls
The mixing of base octylame, and stir evenly, interior phase solution is obtained, it is spare；
External solution is poured into reaction vessel by step 3, and reaction vessel is placed in 40 DEG C of constant temperature water bath, constantly
Stirring；Interior phase solution is slowly dropped into external solution again, so that it is filled mixing, is made into base fluid, leads to the deoxygenation of nitrogen high-speed stirred,
After stirring 40min, 0.5 gram of hydrogen peroxide is slowly added dropwise in reaction vessel and carries out catalysis initiation, sealed reaction vessel, heating
It is cooling to 80 DEG C of isothermal reaction 5h, obtain polymer drag reducer.
Drag reducer is added to the water by step 4, stirring, obtains self-crosslinking height and takes sand cleaning slippery water.
Performance test:
Polymer drag reducer prepared by embodiment 1 is tested for the property.
(1) stability
The drag reducer sample of embodiment 1 is poured into sample bottle, places the steady of different time observation sample itself at room temperature
Qualitative, the results are shown in Table 1.As can be seen that still keeping uniform milky after the drag reducer placed for 5 weeks at room temperature
Liquid condition illustrates that the stability of drag reducer is good.
Table 1, sample stability evaluation
| Standing time | Experimental phenomena |
| 1 day | Uniform milky white liquid |
| 1 week | Uniform milky white liquid |
| 2 weeks | Uniform milky white liquid |
| 3 weeks | Uniform milky white liquid |
| 4 weeks | Uniform milky white liquid |
| 5 weeks | Uniform milky white liquid |
(2) thickening property
Drag reducer prepared by embodiment 1 is added to the water, the slippery water of different drag reducer dosages is configured to, in 25 DEG C of conditions
The viscosity number of the lower various slippery water of test, test result are shown in Table 2.As can be seen that the viscosity of slippery water increases with drag reduction agent content
Add and increase, the thickening property of drag reducer is significant, smooth under conditions of drag reducer dosage is seldom (drag reducer dosage 0.5%)
Water viscosity is up to 72mpa.s.
Viscosity test under table 2, Different adding amount
| Drag reducer dosage, % | Viscosity (25 DEG C), mpa.s |
| 0.05 | 6 |
| 0.1 | 10 |
| 0.2 | 24 |
| 0.3 | 40 |
| 0.4 | 52 |
| 0.5 | 72 |
(3) resistance-reducing yield is tested
The slippery water for preparing drag reduction agent content 0.1%, tests the resistance-reducing yield of drag reducer, test result is shown in Fig. 1.It can see
Out, in slippery water when drag reduction agent content 0.1%, resistance-reducing yield reaches 72% or more.
(4) surface tension is tested
The surface tension for measuring the slippery water of drag reduction agent content 0.1% is 22.78mN/N.
(5) prevent swollen performance test
Dilatancy experiment is carried out to the slippery water of drag reduction agent content 0.1%, test result is shown in Table 3.
Table 3 prevents swollen property test result
| Experimental liquid | Laboratory time (h) | Expansion rate (%) |
| 0.1% slippery water | 2 | 3.34 |
| 0.1% slippery water | 8 | 3.65 |
(6) solid-carrying performance is tested
Sand cleaning slippery water is taken using the self-crosslinking height that drag reducer prepared by embodiment 1 is configured to drag reduction agent content 0.5%.
The slippery water and conventional guanidine gum fracturing fluid (content 0.5%) are subjected to solid-carrying performance test and comparison, the results are shown in Table 4.It can see
Out, the solid-carrying performance that self-crosslinking height of the invention takes sand cleaning slippery water is substantially better than guanidine gum fracturing fluid.
Table 4, two kind of fracturing fluid sand setting speed compare (90 DEG C, 2 hours)
| 20/40 mesh (30%) | Guanidine gum fracturing fluid (0.5%) | Self-crosslinking fracturing fluid (0.5%) |
| Highly (cm) | 9.6 | 5.5 |
| Time (s) | 900 | 900 |
| Sand setting speed (cm/s) | 0.0104 | 0.0061 |
By a series of above-mentioned performance tests, it can be concluded that, self-crosslinking height of the invention, which takes sand cleaning slippery water, has height
Viscosity, sand carrying effect is good, and sand ratio can effectively reduce frictional resistance up to 30%, and solid-carrying performance is excellent, prevents that the swollen and row of helping works well
Advantage.
Application Example
For XX03 well location in Chongqing City, the village Long Mentan, slab bridge town, construction location is that Dongshan north constructs the western wing, the well finishing drilling well depth
6050m, finishing drilling layer position Longma small stream group, using 139.7mm cased hole completion, horizontal segment length 1501.19m designs 32 sections of pressure break, uses
Solvable bridge plug takes sand using self-crosslinking height of the invention as segmentation tool, main body and cleans smooth aqueous systems, using 140Mpa well
Mouth injection, construct pressure limiting 120Mpa.Design parameter is shown in Table 5.The 13rd section of construction curve figure of XX03 well is shown in Fig. 2.(operational discharge capacity 13-
14m3/ min, operation pressure 95-103Mpa, termination of pumping pressure 70Mpa, calculating resistance-reducing yield in construction is 72.05%.
Table 5, XX03 well construction parameter
| Pound sign | Number of segment is transformed | It constructs well section (m) | It constructs segment length (m) | Well logging well temperature |
| XX03 well | 32 | 4490-5991.19 | 1501.19 | 133.5℃/6050.00m |
In conclusion avoiding injury of the fracturing fluid residue to supporting crack to reduce the operating expenses of pressure break, pressure is improved
It splits volume increase effect of well, reduces site operation workload, the present invention develops a kind of novel self-crosslinking height and takes sand cleaning slippery water,
The smooth aqueous systems integrate drop resistance, take sand, prevent the multiple functions such as the swollen, row of helping, and solve conventional slippery water and addition is needed to subtract
The problems such as the various medicaments such as resist, expansion-resisting agent, cleanup additive while sand carrying effect difference.Field application shows that self-crosslinking height is taken
Sand cleaning slippery water can effectively reduce frictional resistance, and solid-carrying performance is excellent, prevents that the swollen and row of helping works well, can be low with other in shale gas
It permeates in the exploitation of fine and close oil-gas reservoir and promotes and applies.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With.It can be applied to various suitable the field of the invention completely.It for those skilled in the art, can be easily
Realize other modification.Therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. a kind of self-crosslinking height take sand cleaning slippery water, which is characterized in that the slippery water be drag reducer is added to the water configuration and
At；The drag reducer is to carry out gathering made of biphasic emulsion polymerization reaction under initiator effect interior phase solution and external solution
Close object lotion；The external solution includes component polyester, green solvent and crosslinking agent；The green solvent is propylene glycol esters
Solvent；The interior phase solution includes component 2- acrylamide-2-methylpro panesulfonic acid, organic amine and water.
2. self-crosslinking height as described in claim 1 takes sand cleaning slippery water, which is characterized in that the matter of the raw material components of drag reducer
It is as follows to measure percentage: polyester 10-15%, green solvent 10-20%, crosslinking agent 1-2%, water 30-45%, 2- acrylamido-
2- methyl propane sulfonic acid 10-20%, organic amine 4-8%, initiator 0.01-0.05%.
3. self-crosslinking height as claimed in claim 2 take sand cleaning slippery water, which is characterized in that the polyester be polyglycolide,
One of polylactide, glycolide-lactide copolymer, polycaprolactone or two kinds of mixture.
4. self-crosslinking height as claimed in claim 2 takes sand cleaning slippery water, which is characterized in that the green solvent is propylene glycol
One of methyl ether acetate, propylene-glycol ethyl ether acetate, propylene glycol butyl ether acetate or at least two kinds of mixture.
5. self-crosslinking height as claimed in claim 2 takes sand cleaning slippery water, which is characterized in that the crosslinking agent is double three ethyl alcohol
One of the double isopropyl zirconates of amine, the double isopropyl zirconic acid ammoniums of dilactic acid, zirconium lactate.
6. self-crosslinking height as claimed in claim 2 takes sand cleaning slippery water, which is characterized in that the organic amine is three second
One of amine, diethyl propylamine, diethyl butylamine, diethylhexylamine, diethyl octylame or diethyl decyl amine or at least two
Mixture.
7. self-crosslinking height as claimed in claim 2 take sand cleaning slippery water, which is characterized in that the initiator be azo,
One of over cure acids or peroxy type free radical initiator.
8. self-crosslinking height as described in claim 1 takes sand cleaning slippery water, which is characterized in that the drag reducer is molecular weight
The polymer emulsion of 500-1000 ten thousand.
9. a kind of self-crosslinking height as described in claim 1~8 any one takes the preparation method of sand cleaning slippery water, feature
It is, includes the following steps:
Step 1 prepares external solution: polyester, green solvent and crosslinking agent being mixed in proportion, stirred evenly, outer mix is obtained
Liquid；
Step 2 prepares interior phase solution: water, 2- acrylamide-2-methylpro panesulfonic acid and organic amine being mixed in proportion, and stirred
It mixes uniformly, obtains interior phase solution, it is spare；
Step 3, biphasic emulsion polymerization: external solution is poured into reaction vessel, reaction vessel is placed in 30~40 DEG C of constant temperature
In water-bath, then interior phase solution is slowly added into external solution by turn on agitator, is uniformly mixed, and nitrogen high-speed stirred is led to
Deoxygenation after stirring 20~40min, initiator is instilled in reaction vessel, sealed reaction vessel is warming up to 80 DEG C of isothermal reactions 4
~5h, it is cooling, obtain drag reducer；
Drag reducer is added to the water by step 4, stirring, obtains self-crosslinking height and takes sand cleaning slippery water.
10. the preparation method that self-crosslinking height as claimed in claim 9 takes sand cleaning slippery water, which is characterized in that drag reducer
The mass percent of raw material components dosage is as follows: polyester 10-15%, green solvent 10-20%, crosslinking agent 1-2%, water 30-
45%, 2- acrylamide-2-methylpro panesulfonic acid 10-20%, organic amine 4-8%, initiator 0.01-0.05%.
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| CN102977877A (en) * | 2012-12-04 | 2013-03-20 | 西南石油大学 | Drag reducer for shale gas fracture and preparation method of drag reducer |
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2019
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|---|---|---|---|---|
| CN102977877A (en) * | 2012-12-04 | 2013-03-20 | 西南石油大学 | Drag reducer for shale gas fracture and preparation method of drag reducer |
| CN107964399A (en) * | 2017-11-23 | 2018-04-27 | 北京捷贝通石油技术股份有限公司 | A kind of shale gas pressure break multifunctional nano lotion drag reducer and preparation method thereof |
| CN108192587A (en) * | 2017-12-19 | 2018-06-22 | 北京捷贝通石油技术有限公司 | A kind of shale gas pressure break multifunctional cleaning drag reducer and preparation method thereof |
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