CN104774605A - Low damage small molecule environmental-protection type fracturing fluid and preparation method thereof - Google Patents

Low damage small molecule environmental-protection type fracturing fluid and preparation method thereof Download PDF

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Publication number
CN104774605A
CN104774605A CN201410012079.XA CN201410012079A CN104774605A CN 104774605 A CN104774605 A CN 104774605A CN 201410012079 A CN201410012079 A CN 201410012079A CN 104774605 A CN104774605 A CN 104774605A
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China
Prior art keywords
fracturing fluid
small molecules
cross
guar gum
environmentally
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Pending
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CN201410012079.XA
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Chinese (zh)
Inventor
王丹
黄波
仲岩磊
姜阿娜
李爱山
钟安海
陈凯
陈磊
鞠玉芹
宋李煜
刘霜
杨彪
吕永利
冯绍云
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China Petroleum and Chemical Corp
Oil Production Technology Research Institute of Sinopec Shengli Oilfield Co
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China Petroleum and Chemical Corp
Oil Production Technology Research Institute of Sinopec Shengli Oilfield Co
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Priority to CN201410012079.XA priority Critical patent/CN104774605A/en
Publication of CN104774605A publication Critical patent/CN104774605A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/62—Compositions for forming crevices or fractures
    • C09K8/66—Compositions based on water or polar solvents
    • C09K8/68—Compositions based on water or polar solvents containing organic compounds
    • C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • 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
    • C09K8/84—Compositions based on water or polar solvents
    • C09K8/86—Compositions based on water or polar solvents containing organic compounds
    • C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
    • C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention provides a low damage small molecule environmental-protection type fracturing fluid and a preparation method thereof. The fracturing fluid comprises 100 parts by weight of a base liquid and 0.5-0.8 part by weight of an organic boron cross-linking agent, wherein the base liquid comprises a low molecular guar gum, a cleanup additive, a clay stabilizer, a pH value adjuster, a sterilizing agent and water, and the organic boron cross-linking agent is obtained by mixing a borate and a NaOH aqueous solution according to a certain ratio. The preparation method comprises: preparing the low molecular weight guar gum and the organic boron cross-linking agent, and carrying out cross-linking on the base liquid and the cross-linking agent according to a certain cross-linking ratio to prepare a jelly fracturing fluid, wherein the viscosity is more than or equal to 50 mpa.s after the obtained fracturing fluid is sheared for 2 h at a temperature of 120 DEG C and a shear rate of 170 s<-1>, the lowest core matrix injury rate is 15%, the lowest residue content is 116 mg/L, and the fracturing fluid being subjected to gel breaking can be reused after the pH value is re-adjusted, such that the fracturing fluid of the present invention is the environmental protection fracturing fluid system.

Description

A kind of Low Damage small molecules environmentally-friendly fracturing fluid and preparation method thereof
Technical field
The present invention relates to oil-gas field development technical field, be specifically related to a kind of Low Damage small molecules environmentally-friendly fracturing fluid and preparation method thereof.
Background technology
The effective exploitation of oil field ultra-permeable reservior mainly relies on fracturing technique, and fracturing liquid is important component part and the key link of fracturing reform, has certain temperature and shearing sustainability, and the fracturing liquid of low residue Low Damage is the focus of current fracturing liquid research.
Guar gum fracturing fluid is applied for many years in oil field due to its cheap cost and good temperature and shearing sustainability thereof, but the feature of its vegetable jelly makes its residue content higher, and formation injury is comparatively large, more outstanding for this impact of vulnerable reservoir.Patent " a kind of Low Damage small molecules guar gum fracturing fluid " ZL201110263461.4, relate to a kind of Low Damage small molecules guar gum fracturing fluid be made up of base fluid and gel breaker, linking agent, effectively reduce the injury of fracturing liquid formation, improve the effect of fracturing reform.
We consider with low molecule melon glue for reaction raw materials prepares a kind of low molecular weight fracturing fluids for low permeability oil field, this fracturing fluid system has the rheological of conventional crosslinked polymer fluid, there is low residue Low Damage performance simultaneously, do not need gel breaker, be cross-linked and controlled by pH, possess the crosslinked stream of natural boron and become reversibility, after pressure under the neutralizing effect on stratum, reduce fracturing liquid pH value, realize brokenly glue object.
Summary of the invention
The object of the present invention is to provide a kind of Low Damage small molecules environmentally-friendly fracturing fluid and preparation method thereof, this fracturing liquid has the rheological of conventional crosslinked polymer fluid, has low residue Low Damage performance simultaneously, does not need to use gel breaker, can reuse, be a kind of environmentally-friendly fracturing fluid.
In order to reach above-mentioned purpose, an object of the present invention realizes by following technical measures:
A kind of Low Damage small molecules environmentally-friendly fracturing fluid, be made up of the base fluid of 100 weight parts and the organic borate cross-linker of 0.5-0.8 weight part, it is characterized in that, described base fluid is made up of the raw material of following weight:
Low molecule guar gum 0.3-0.6 cleanup additive 0.3-0.5 clay stabilizer 0.3-0.5
PH adjusting agent appropriate disinfectant 0.03-0.1 high-temperature stabiliser 0.1-0.3
Water 98-99;
Described organic borate cross-linker is by borate and 10-30%(mass concentration) the NaOH aqueous solution is in 100:5-100:10(weight part) ratio be mixed to get.
Described small molecules guar gum refers to that molecular weight is the modifyed guar gum of 30-40 ten thousand, its preparation process is: by guar gum or hydroxypropylguar gum and water by 10-15(weight part): 1000(parts by volume) proportioning obtain the aqueous solution, the above-mentioned aqueous solution of mannosans enzyme liberating to the viscosity adding 0.1-0.5g/L is between 20-40mPa.s, then the 80-90 DEG C of enzyme that goes out is warming up to, reaction stops, finally this aqueous solution G2# sand core funnel is filtered also lyophilization, pulverizing obtained Powdered low molecule viscosifying agent, i.e. small molecules guar gum;
Described cleanup additive is Trimethyllaurylammonium bromide or cetyl trimethylammonium bromide;
Described clay stabilizer is KCl, NH 4cl or cation quaternary ammonium salt base polymer;
Described pH adjusting agent is Na 2cO 3, NaHCO 3or NaOH;
Described disinfectant is formaldehyde or glutaraldehyde;
Described high-temperature stabiliser is Na 2s 2o 3.
Described borate is containing poly-hydroxy ligand L 1, L 2, ligand L 1for polyvinyl alcohol, ligand L 2for glycerine;
Two of object of the present invention realizes by following technical measures:
Prepare a method for Low Damage small molecules environmentally-friendly fracturing fluid, carry out as follows:
By above-mentioned weight, low molecule guar gum, cleanup additive, clay stabilizer is added in water, high-temperature stabiliser, pH adjusting agent is adopted to regulate pH to be 10-12, add disinfectant again, be then cross-linked and obtain frozen glue shape fracturing liquid with obtained organic borate cross-linker with the crosslinking ratio of 100:0.5-100:0.8.
Compared with prior art, beneficial effect of the present invention is, the more concentrated high-temperature stabiliser that adds of small molecules melon xanthan molecule amount distribution obtained improves of the fracturing fluid temperature tolerance, small molecules melon glue had not only been taken into account of the fracturing fluid temperature and shearing sustainability but also can have been effectively reduced the injury of fracturing liquid formation, without the need to gel breaker, and can reuse, be a kind of environment-friendly type pressure break system.This fracturing liquid ties up to 120 DEG C, 170s -1shearing rate down cut 2h, viscosity is at more than 50mpa.s; It is to rock core matrix damage rate minimum 15%, the minimum 116mg/L of residue content; Fracturing liquid 100 DEG C, the 170s of secondary crosslinking after crosslinked and broken glue first -1shearing rate down cut 1.5h, viscosity, all at more than 50mpa.s, can reuse.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 fracturing liquid is at 100 DEG C, 170s -1resistant to shearing graphic representation under shearing rate.
Fig. 2 is that the embodiment of the present invention 2 fracturing liquid is at 120 DEG C, 170s -1resistant to shearing graphic representation under shearing rate.
Fig. 3 be cross-linked first and after broken glue the embodiment fracturing liquid of secondary crosslinking at 100 DEG C, 170s -1resistant to shearing graphic representation under shearing rate.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
Step one: prepare small molecules guar gum
By guar gum with water in 10(weight part): 1000(parts by volume) ratio mix the obtained aqueous solution, the above-mentioned aqueous solution of mannosans enzyme liberating to the viscosity adding 0.1g/L is 20mPa.s, then 80 DEG C of enzymes that go out are warming up to, reaction stops, and is finally filtered by this aqueous solution G2# sand core funnel and lyophilization, the obtained Powdered small molecules guar gum of pulverizing.
Step 2: prepare organic borate cross-linker
The NaOH aqueous solution of borate and 10% mass concentration is mixed to get organic borate cross-linker by the weight ratio of 100:5.
Step 3: prepare Low Damage small molecules environmentally-friendly fracturing fluid
Powdered small molecules guar gum, the Trimethyllaurylammonium bromide of 0.3 weight part, the KCl of 0.3 weight part of 0.3 weight part step one preparation is added in the water of 99 weight parts, pH adjusting agent NaOH is adopted to regulate pH to be 10, add the formaldehyde of 0.03 weight part again, be then cross-linked and obtain frozen glue shape fracturing liquid with the organic borate cross-linker of 0.5 obtained weight part with the crosslinking ratio of 100:0.5.With HAKKE rheometer test frozen glue rheological property at 100 DEG C, 170s -1after shearing 120min, viscosity remains on more than 50mPa.s, and data are shown in Fig. 1.
Embodiment 2
Step one: prepare small molecules guar gum
By hydroxypropylguar gum with water in 15(weight part): 1000(parts by volume) ratio mix the obtained aqueous solution, the above-mentioned aqueous solution of mannosans enzyme liberating to the viscosity adding 0.5g/L is 40mPa.s, then 90 DEG C of enzymes that go out are warming up to, reaction stops, and is finally filtered by this aqueous solution G2# sand core funnel and lyophilization, the obtained Powdered small molecules guar gum of pulverizing.
Step 2: prepare organic borate cross-linker
The NaOH aqueous solution of borate and 30% mass concentration is mixed to get organic borate cross-linker by the weight ratio of 100:10.
Step 3: prepare Low Damage small molecules environmentally-friendly fracturing fluid
The Powdered small molecules guar gum of 0.6 weight part step one preparation, the Trimethyllaurylammonium bromide of 0.5 weight part, the KCl of 0.5 weight part, the Na of 0.2 weight part is added in the water of 98 weight parts 2s 2o 3, adopt pH adjusting agent NaOH to regulate pH to be 12, then add the formaldehyde of 0.1 weight part, be then cross-linked and obtain frozen glue shape fracturing liquid with the organic borate cross-linker of 0.8 obtained weight part with the crosslinking ratio of 100:0.8.With HAKKE rheometer test frozen glue rheological property at 120 DEG C, 170s -1after shearing 120min, viscosity remains on more than 50mPa.s, and data are shown in Fig. 2.
Embodiment 3
As embodiment 1 and 2, difference is, Trimethyllaurylammonium bromide adopts cetyl trimethylammonium bromide to replace.
Embodiment 4
As embodiment 1 and 2, difference is, KCl adopts NH 4cl or cation quaternary ammonium salt base polymer replace.
Embodiment 5
As embodiment 1 and 2, difference is, pH adjusting agent adopts Na 2cO 3replace.
Embodiment 6
As embodiment 1 and 2, difference is, formaldehyde adopts glutaraldehyde to replace.
By fracturing liquid establishing criteria (the aqueous fracturing fluid performance evaluation that above-described embodiment is prepared, SY-T5107-2005,6.10th, 6.14) test it to matrix permeability of rock core injury and remaining solid level of residue after breaking glue, injury data are as shown in following table 1.Conventional fracturing liquid is to core damage rate more than 25%, and more than residue content 200mg/L, contrasts thus, and fracturing fluid system of the present invention is a kind of low damage fracture liquid system.
table 1 residue and injury rate experimental result
Numbering Residue content (mg/L) Injury rate (%)
Embodiment 1 127 17
Embodiment 2 116 25
Embodiment 3 193 18
Embodiment 4 122 19
Embodiment 5 154 15
Embodiment 6 133 20
Fig. 3 is 100 DEG C, 170s -1the flow curve of surveying under condition, blue curve is the fracturing liquid of first preparation, and shear through 90min, viscosity remains on 200mPas.Red curve be add pulverize capsule acid after 90 DEG C of broken glue 2h, add Na 2cO 3flow curve after adjust ph.As can be seen from the figure, equally after 90min shears, fracturing liquid viscosity also remains on 85mPas.This illustrates that readjusting pH value after this small molecules guar gum fracturing fluid system breaks glue can reuse, and is a kind of environmentally-friendly fracturing fluid system.

Claims (7)

1. a Low Damage small molecules environmentally-friendly fracturing fluid, be made up of the base fluid of 100 weight parts and the organic borate cross-linker of 0.5-0.8 weight part, it is characterized in that, described base fluid is made up of the raw material of following weight:
Low molecule guar gum 0.3-0.6 cleanup additive 0.3-0.5 clay stabilizer 0.3-0.5
Disinfectant 0.03-0.1 water 98-99;
Described organic borate cross-linker is by borate and 10-30%(mass concentration) the NaOH aqueous solution is in 100:5-100:10(weight part) ratio be mixed to get.
2. a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, it is characterized in that, the preparation process of described low molecule guar gum is:
By guar gum or hydroxypropylguar gum and water by 10-15(weight part): 1000(parts by volume) proportioning obtain the aqueous solution, the above-mentioned aqueous solution of mannosans enzyme liberating to the viscosity adding 0.1-0.5g/L is between 20-40mPa.s, then the 80-90 DEG C of enzyme that goes out is warming up to, reaction stops, finally this aqueous solution G2# sand core funnel is filtered also lyophilization, pulverizing obtained Powdered low molecule viscosifying agent, i.e. low molecule guar gum.
3. a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, it is characterized in that, described cleanup additive is Trimethyllaurylammonium bromide or cetyl trimethylammonium bromide.
4. a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, it is characterized in that, described clay stabilizer is KCl, NH 4cl or cation quaternary ammonium salt base polymer.
5. a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, it is characterized in that, described disinfectant is formaldehyde or glutaraldehyde.
6. a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, is characterized in that, described borate is containing poly-hydroxy ligand L 1, L2, and ligand L 1 is polyvinyl alcohol, and ligand L 2 is glycerine.
7. prepare the method for a kind of Low Damage small molecules environmentally-friendly fracturing fluid as claimed in claim 1, it is characterized in that, carry out as follows:
Add low molecule guar gum, cleanup additive, clay stabilizer in water, adopt pH adjusting agent to regulate pH to be 10-12, then add disinfectant, be then cross-linked and obtain frozen glue shape fracturing liquid with obtained organic borate cross-linker.
CN201410012079.XA 2014-01-11 2014-01-11 Low damage small molecule environmental-protection type fracturing fluid and preparation method thereof Pending CN104774605A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105586026A (en) * 2015-07-28 2016-05-18 陕西太昱科技发展有限公司 Biologically recyclable biogum oil well fracturing fluid and preparation method thereof
CN106467590A (en) * 2015-08-21 2017-03-01 中国石油化工股份有限公司 A kind of pressure break preparation method of SOLID ORGANIC borate crosslinker
CN110079292A (en) * 2019-03-22 2019-08-02 中国石油化工股份有限公司 High-content wax oil reservoir fracturing composition, high-content wax oil reservoir fracturing fluid and high-content wax oil reservoir composite fracturing fluid
CN110551494A (en) * 2018-06-04 2019-12-10 深圳市百勤石油技术有限公司 Composite water-based fracturing fluid for fracturing yield-increasing measures and preparation method thereof

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CN102757779A (en) * 2012-07-10 2012-10-31 陕西科技大学 Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum
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CN102329603B (en) * 2011-08-03 2013-01-30 西安长庆化工集团有限公司 Low-concentration carboxymethyl fracturing fluid and preparation method thereof
CN102352233A (en) * 2011-09-07 2012-02-15 西南石油大学 Low-harm micro-molecular guar gum fracturing fluid
CN102757779A (en) * 2012-07-10 2012-10-31 陕西科技大学 Preparation method of acidic crosslinking agent applied to carboxymethyl guar gum

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105586026A (en) * 2015-07-28 2016-05-18 陕西太昱科技发展有限公司 Biologically recyclable biogum oil well fracturing fluid and preparation method thereof
CN106467590A (en) * 2015-08-21 2017-03-01 中国石油化工股份有限公司 A kind of pressure break preparation method of SOLID ORGANIC borate crosslinker
CN110551494A (en) * 2018-06-04 2019-12-10 深圳市百勤石油技术有限公司 Composite water-based fracturing fluid for fracturing yield-increasing measures and preparation method thereof
CN110079292A (en) * 2019-03-22 2019-08-02 中国石油化工股份有限公司 High-content wax oil reservoir fracturing composition, high-content wax oil reservoir fracturing fluid and high-content wax oil reservoir composite fracturing fluid

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Application publication date: 20150715