CN102226080A - Breakdown fluid and preparation method thereof - Google Patents
Breakdown fluid and preparation method thereof Download PDFInfo
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- CN102226080A CN102226080A CN2011101053110A CN201110105311A CN102226080A CN 102226080 A CN102226080 A CN 102226080A CN 2011101053110 A CN2011101053110 A CN 2011101053110A CN 201110105311 A CN201110105311 A CN 201110105311A CN 102226080 A CN102226080 A CN 102226080A
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Abstract
The invention relates to a breakdown fluid and a preparation method thereof. The breakdown fluid comprises the following components: thickener 0.3-1.2%, clay stabilizer 0.5-2%, bactericide 0.01-0.2%, cleanup additive 0.2-1%, and the balance of water-borne working fluid, wherein the thickener is a betaine-type amphoteric thickener based on guar gum derivatives and has a structural formula (I): wherein R is selected from hydroxylpropyl group, hydroxyethyl group, carboxymethyl group and 2-hydroxylpropyl-N,N,N-trimethyl group; R1 and R2 independently represent C1-C4 alkyl group, R3 represents carboxylate radical COO<-> or sulfonate radical SO3<->; and the degree of substitution of R is 0.02-0.6, and the degree of substitution of the betaine type amphoteric ions is 0.02-0.6.
Description
Technical field
The present invention relates to a kind of fracturing liquid and preparation method thereof.
Background technology
Waterfrac treatment is one of main offensive measure of low-permeability oilfield hydrocarbon zone transformation, present employed melon glue or hydroxypropyl melon fracturing fluid mostly are fresh water base fracturing liquid, few or need for strong well under the situation of high salinity high-density aqueous fracturing fluid for the offshore oilfield Freshwater resources, this fracturing liquid ties up in the seawater of high ionic strength, easily produce the shrink phenomenon and reduce fracturing liquid viscosity, thereby influence of the fracturing fluid prop-carrying capacity, reduce the fracturing liquid result of use, the techno-economic effect variation is difficult to satisfy the needs of pressing crack construction.
Therefore, need a kind of improved fracturing liquid that is applicable to multiple water base working fluid.
Summary of the invention
Primary and foremost purpose of the present invention provides a kind of fracturing liquid.
Another object of the present invention provides a kind of of the fracturing fluid preparation method.
Fracturing liquid of the present invention comprises the thickening material of 0.3%-1.2%, the clay stabilizer of 0.5%-2%, the sterilant of 0.01%-0.2%, the cleanup additive of 0.2%-1%, surplus is water base working fluid, wherein said thickening material is the betaine type amphoteric thickening material based on guar gum derivative, and it has structural formula (I):
(I)
Wherein R is selected from hydroxypropyl, hydroxyethyl, carboxymethyl, 2-hydroxypropyl-N, N, N-trimethylammonium, R
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical COO
-Or sulfonate radical SO
3 -The R substitution value is (0.02～0.6), and betaine type amphoteric ion pair substitution value is (0.02～0.6).
Preferably, total substitution value is (0.03～0.8).
Clay stabilizer can be this area clay stabilizer commonly used, as is selected from Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC) or Repone K; Cleanup additive can be this area cleanup additive commonly used, as is selected from FN-2 (fluorine-containing ether acid amide type tertiary amine oxide) or alkylphenol polyoxyethylene, and they all originate from COSL Chemicals (Tianjin) Co., Ltd.; Sterilant can be this area sterilant commonly used, as is selected from formaldehyde or Trimethyllaurylammonium bromide, and they are by commercial acquisition.
In another embodiment, fracturing liquid of the present invention also comprises the linking agent of 0.1%-3%.Linking agent is selected from sodium tetraborate, polyvalent alcohol boric acid fat, titanium tetrachloride, basic zirconium chloride, the two sec.-propyl titanium acid ammoniums of dilactic acid and methyl ethyl diketone zirconic acid fat.
The invention still further relates to the of the fracturing fluid method of a kind of preparation, it comprises the steps:
A. at first prepare thickening material;
1) pre-treatment melon collagen powder;
2) be 2-3 with weight ratio: 1 solvent mix with pretreated melon collagen powder melon colloidal suspension liquid; The phase-transfer catalyst that adds the 0.01wt%-2wt% of described melon colloidal suspension liquid gross weight;
3) stir and be warming up to 30-40 ℃;
4) add alkali lye and alkalization;
5) after alkalization finished, the dropping mol ratio was ampholytic ion pair monomer and the etherifying agent of 0.1-1: 1-0.1, and adds described alkali lye again;
6) be warming up to 50 ℃-70 ℃, reacted 4-6 hour;
7) after reaction finished, washing, drying, pulverizing promptly got thickening material of the present invention;
Wherein zwitter-ion is to being:
R wherein
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical COO
-Or sulfonate radical SO
3 -Wherein etherifying agent is selected from propylene oxide, chloroethanol, sodium chloroacetate and 3-chloro-2-hydroxypropyl-N, N, N-trimethyl ammonium chloride; Wherein alkali lye is taken from the aqueous solution of sodium hydroxide or yellow soda ash; With
B. prepared thickening material is mixed according to described amount with clay stabilizer, sterilant, cleanup additive and promptly get fracturing liquid.
In another embodiment, the of the fracturing fluid preparation method of the present invention comprises the steps:
A. at first prepare thickening material;
1) pre-treatment melon collagen powder;
2) be 2-3 with weight ratio: 1 solvent mix with pretreated melon collagen powder the melon sol solution; The phase-transfer catalyst that adds the 0.01wt%-2wt% of described melon sol solution gross weight;
3) stir and be warming up to 30-40 ℃;
4) add alkali lye and alkalization;
5) after alkalization finished, the dropping mol ratio was ampholytic ion pair monomer and the etherifying agent of 0.1-1: 1-0.1, and adds described alkali lye again;
6, be warming up to 50 ℃-70 ℃, reacted 4-6 hour;
7, after reaction finished, washing, drying, pulverizing promptly got thickening material of the present invention;
Wherein zwitter-ion is to being:
R wherein
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical-COO
-Or sulfonate radical-SO
3 -Wherein etherifying agent is selected from propylene oxide, chloroethanol, sodium chloroacetate and 3-chloro-2-hydroxypropyl-N, N, N-trimethyl ammonium chloride; Wherein alkali lye is taken from the aqueous solution of sodium hydroxide or yellow soda ash; With
B. according to described amount with thickening material mix with clay stabilizer, sterilant, cleanup additive base fluid, and then add linking agent and carry out crosslinking reaction and promptly get fracturing liquid.
The phase-transfer catalyst that uses in the inventive method can be selected this area tensio-active agent commonly used, as long as it plays solubilising and osmosis, preferred palmityl trimethyl ammonium chloride, 16 octadecyl trimethyl ammonium chloride, 14 palmityl trimethyl ammonium chlorides etc.
The solvent that uses in the inventive method as this area commonly used can be miscible with water alcohol, as the mixing solutions with water such as methyl alcohol, ethanol, propyl alcohol, preferred volume ratio is the mixing solutions of 4: 1 second alcohol and water.
As used herein, term " water base working fluid " refers to the water base and saline based working fluid through fresh water base, seawater base, the stratum of fine filtering.
During use, the crosslinked beguine of base fluid and linking agent is according to linking agent kind and the different actual modulated of carrying out of concentration.As when adopting borax as the linking agent preparing fracturing fluid, compound method can be as follows:
The first step: thickening material is dissolved in the seawater, is mixed with base fluid, regulate PH=8～12 with soda ash or caustic soda by concentration 0.6%～1.0%, swelling 1～4 hour, dissolving evenly back is stand-by.
Second step: the preparation crosslinked fluid: borax is by concentration 2% dosage, ammonium persulphate (gel breaker) is by concentration 0.1%～1% dosage, add 0.1～0.5% cleanup additive, 1～2% clay stabilizer according to the oil reservoir situation simultaneously, 0.1% sterilant etc., even with the seawater dissolving, thus be mixed with a certain amount of crosslinked fluid.
The 3rd step: in pressure break infusion process, adjust pumping rate, by crosslinked than (base fluid: crosslinked fluid)=100: 10 (transfer hang up be as the criterion) pump into base fluid and crosslinked fluid, and add fracturing sand, 0.002%～0.2% ammonium persulphate (or capsule ammonium persulphate, benzoyl peroxide) etc. than (20～60%) gradient according to design sand.
The 4th step: construction finishes closing well, step-down, discharge opeing, operation.
The present invention introduces polar group and has improved the solvability of melon glue in seawater (or salt solution), and the shielding effect of gegenion in the seawater (or salt solution), then improved the thickening power of amphoteric guar gum in seawater, suppressed the coagulation phenomenon of guar gum in seawater (or salt solution), improved adaptive faculty and the heat resistance of guar gum gel in seawater (or salt solution), form the shear-stable gelinite, have good prop-carrying capacity, anti-shear performance and temperature tolerance.When existing, the fracturing liquid performance can satisfy the needs of waterfrac treatment engineering under 60 ℃～180 ℃ hydrocarbon zone conditions at high-temperature stabiliser (Sulfothiorine, thiocarbamide, aniline etc.).
Fracturing liquid system based on guar derivative of the present invention, can realize satisfying marine pressing crack construction needs with the seawater preparing fracturing fluid, also can be used for preparing high salinity, high-density (being equivalent to 35% normal saline solution) aqueous fracturing fluid, to reduce, satisfy the needs of deep well high pressure stratafrac to the waterfrac treatment power demand.
Fracturing liquid plays the effect of transmitting energy, taking sand and making seam in oil gas well and the waterfrac treatment of coal gas layer.Concrete of the fracturing fluid on-site preparation should carry out corresponding allotment according to formation condition (temperature, formation lithology etc.), to satisfy FRACTURING DESIGN to rheological and take the requirement of sand.
The accompanying drawing summary
Fig. 1 has shown the of the fracturing fluid rheological of preparing based on melon collagen powder in the prior art of seawater base; With
Fig. 2 has shown the of the fracturing fluid rheological of seawater base based on the guar gum derivative preparation of the inventive method.
Embodiment
The present invention will be further described below in conjunction with embodiment, the material that adopts in following examples, and except indicating, all the other are commercially available.
Embodiment 1:
A. prepare thickening material earlier, step is as follows:
1, with the pre-treatment under high-temperature steam of melon collagen powder;
2, the mixed solvent (volume ratio 4: 1) with 50 liters second alcohol and water pumps in the reactor, starts stirrer, slowly adds 15kg melon collagen powder (sheet); Add the 0.1kg palmityl trimethyl ammonium chloride again as phase-transfer catalyst;
3, stirring and intensification rise to 30 ℃-40 ℃ with 1 ℃ of-3 ℃/min of temperature rise rate;
4, pump into 0.9kg NaOH and 2.5 liters of H
2O alkalized 30 minutes;
5, after alkalization finishes, drip ion pair monomer 3-chloro-2-hydroxypropyl-N of 11.55kg, the propylene oxide of N-dimethyl-sultaine and 2.85kg (mol ratio 1: 1) pumps into 0.9kg NaOH and 2.5 liters of H
2O;
6, rise to 50 ℃～70 ℃ with 1 ℃ of-3 ℃/min of temperature rise rate, reacted 4-6 hour;
7, after reaction finishes, dry then, pulverize with Glacial acetic acid and washing with alcohol, promptly get the thickening material of following formula:
B. measuring the 300ml seawater with graduated cylinder pours in the beaker that has magnetic stirring apparatus, start agitator and stir with about 500rpm rotating speed, under normal temperature condition, add 0.6g cleanup additive FN-2,6g Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC), 0.3g formaldehyde then successively, slowly add the prepared thickening material of 1.95g at last again, treat swelling back (about 30 minutes) fully, promptly get fracturing liquid.
Embodiment 2:
A. prepare thickening material earlier, step is as follows:
1, with the pre-treatment under high-temperature steam of melon collagen powder;
2, the mixed solvent (volume ratio 4: 1) with 50 liters second alcohol and water pumps in the reactor, starts stirrer, slowly adds 15Kg melon collagen powder (sheet).Add the 0.1kg palmityl trimethyl ammonium chloride as phase-transfer catalyst;
3, stirring and intensification rise to 30 ℃～40 ℃ with 1 ℃ of temperature rise rate～3 ℃/min;
4, pump into 0.9kg NaOH and 2.5 liters of H
2O, and alkalized 30 minutes;
5, after alkalization finishes, drip ion pair monomer 3-chloro-2-hydroxypropyl-N of 9.75kg, N-dimethyl-carboxybetaine and 4.0kg chloroethanol (mol ratio 1: 1) pump into 0.9kg NaOH and 2.5 liters of H
2O;
6, rise to 50 ℃～70 ℃ with 1 ℃ of temperature rise rate～3 ℃/min, reacted 4～6 hours;
7, after reaction finishes, dry then, pulverize with Glacial acetic acid and washing with alcohol, promptly get the thickening material of following formula:
B. measuring the 300ml seawater with graduated cylinder pours in the beaker that has magnetic stirring apparatus, start agitator and stir with about 500rpm rotating speed, under normal temperature condition, add 0.6g cleanup additive FN-2 then successively, 6g Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC), 0.3g formaldehyde, slowly add the prepared thickening material of 1.95g at last again, treat swelling back (about 30 minutes) fully, adding soda ash in beaker makes pH value in the scope of 9-12, slowly the borax solution that adds about 1.5g then, reaction continues to and makes the fracturing liquid that is mixed with have good visco-elasticity, can hang with glass stick and be advisable.
Embodiment 3:
A. prepare thickening material earlier, step is as follows:
1, with the pre-treatment under high-temperature steam of melon collagen powder;
2, the mixed solvent (volume ratio 4: 1) with 50 liters second alcohol and water pumps in the reactor, starts stirrer, slowly adds 15Kg melon collagen powder (sheet); Add the 0.1kg palmityl trimethyl ammonium chloride as phase-transfer catalyst;
3, stirring and intensification rise to 30 ℃～40 ℃ with 1 ℃ of temperature rise rate～3 ℃/min;
4, pump into 0.9kg NaOH and 2.5 liters of H
2O, and alkalized certain 30 minutes;
5, after alkalization finishes, drip the ion pair monomer 2 of 9.42kg, 3-epoxypropyl-N, the sodium chloroacetate aqueous solution of N-dimethyl-sultaine and 4.7kg (mol ratio 1: 1) pumps into 0.9kg NaOH and 2.5 liters of H
2O.
6, rise to 50 ℃～70 ℃ with 1 ℃ of temperature rise rate～3 ℃/min, reacted 3～5 hours;
7, after reaction finishes, dry then, pulverize with Glacial acetic acid and washing with alcohol, promptly get the thickening material of following formula:
B. measuring the 300ml seawater with graduated cylinder pours in the beaker that has magnetic stirring apparatus, start agitator and stir with about 500rpm rotating speed, under normal temperature condition, add 0.6g cleanup additive FN-2,6g Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC), 0.3g formaldehyde then successively, slowly add the prepared thickening material of 1.95g at last again, treat swelling back (about 30 minutes) fully, promptly get fracturing liquid.
Embodiment 4:
A. prepare thickening material earlier, step is as follows:
1, with the pre-treatment under high-temperature steam of melon collagen powder;
2, the mixed solvent (volume ratio 4: 1) with 50 liters second alcohol and water pumps in the reactor, starts stirrer, slowly adds 15Kg melon collagen powder (sheet); Add the 0.1kg palmityl trimethyl ammonium chloride as phase-transfer catalyst;
3, stirring and intensification rise to 30 ℃～40 ℃ with 1 ℃ of temperature rise rate～3 ℃/min;
4, pump into 0.9kg NaOH and 2.5 liters of H
2O, and alkalized 30 minutes;
5, after alkalization finishes, drip the ion pair monomer 2 of 7.95kg, 3-epoxypropyl-N, 3-chloro-2-hydroxypropyl-N of N-dimethyl-carboxybetaine and 9.4kg, N, the N-trimethyl ammonium chloride pumps into 0.9kgNaOH and 2.5 liters of H again
2O;
6, rise to 50 ℃～70 ℃ with 1 ℃ of temperature rise rate～3 ℃/min, reacted 3～5 hours;
7, after reaction finishes, dry then, pulverize with Glacial acetic acid and washing with alcohol, promptly get the thickening material of following formula:
B. measuring the 300ml seawater with graduated cylinder pours in the beaker that has magnetic stirring apparatus, start agitator and stir with about 500rpm rotating speed, under normal temperature condition, add 0.6g cleanup additive FN-2 then successively, 6g Poly Dimethyl Diallyl Ammonium Chloride (PDMDAAC), 0.3g formaldehyde, slowly add the prepared thickening material of 1.95g at last again, treat swelling back (about 30 minutes) fully, adding soda ash in beaker makes pH value in the scope of 9-12, slowly the borax solution that adds about 1.5g then, reaction continues to and makes the fracturing liquid that is mixed with have good visco-elasticity, can hang with glass stick and be advisable.
Performance evaluation:
According to SY/T 5107-2005 aqueous fracturing fluid method of evaluating performance fracturing liquid of the present invention is carried out performance evaluation.
Following table 1 has shown fracturing liquid and the performance index of fracturing liquid of the prior art in seawater that made by embodiment 1.
Table 1
| Project | The fracturing liquid of embodiment 1 preparation | The fracturing liquid of prior art for preparing | Remarks |
| Base fluid apparent viscosity (mPa.s) | ?60 | 90 | Normal temperature, 170s-1, |
| Fracturing fluid residue (mg/m 3) | ?222 | 1080 | |
| Preparation digestion time (min) | Less than 10 | Greater than 240 |
As can be seen from Table 1, compare, shorten greatly by the embodiment 1 preparation of the fracturing fluid preparation time, help on-the-spot quick dosing like this with the fracturing liquid of prior art; Secondly, because the fracturing fluid residue content of the embodiment of the invention 1 is low than the fracturing liquid of prior art, can reduce the injury of fracturing liquid greatly like this to the stratum.
Fig. 1 is the flow curve of the thickening material based on melon collagen powder+0.5% boroglyceride+seawater of 0.6%; Fig. 2 is the flow curve of the thickening material based on guar gum derivative+0.5% boroglyceride+seawater of making among 0.6% the embodiment 1.Can see that by the flow curve of Fig. 2 of the fracturing fluid structural strength that embodiment 1 makes is better than in the prior art that Fig. 1 shows the fracturing liquid based on melon collagen powder, show good temperature resistance anti-shear performance, 115 ℃ of condition down cuts 120 minutes, viscosity remains on more than the 110mPa.s, and fracturing liquid of the prior art is 115 ℃ of condition down cuts 50 minutes, and viscosity just is reduced to below the 50mPa.s.
Being the preferred embodiments of the present invention only below, is not to be used to limit protection scope of the present invention, therefore, all any modifications of being done within the spirit and principles in the present invention, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. fracturing liquid, comprise the thickening material of 0.3%-1.2%, the clay stabilizer of 0.5%-2%, the sterilant of 0.01%-0.2%, the cleanup additive of 0.2%-1%, surplus is water base working fluid, wherein said thickening material is the betaine type amphoteric thickening material based on guar gum derivative, and it has structural formula (I):
Wherein R is selected from hydroxypropyl, hydroxyethyl, carboxymethyl and 2-hydroxypropyl-N, N, N-trimethylammonium; R
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical COO
-Or sulfonate radical SO
3 -The R substitution value is (0.02～0.6), and betaine type amphoteric ion pair substitution value is (0.02～0.6).
2. fracturing liquid as claimed in claim 1 also comprises the linking agent of 0.1%-3%.
3. fracturing liquid as claimed in claim 2, wherein said linking agent are selected from sodium tetraborate, polyvalent alcohol boric acid fat, titanium tetrachloride, basic zirconium chloride, the two sec.-propyl titanium acid ammoniums of dilactic acid and methyl ethyl diketone zirconic acid fat.
4. one kind prepares of the fracturing fluid method as claimed in claim 1, and it comprises the steps:
A. at first prepare thickening material;
1) pre-treatment melon collagen powder;
2) be 2-3 with weight ratio: 1 solvent mix with pretreated melon collagen powder melon colloidal suspension liquid; The phase-transfer catalyst that adds the 0.01wt%-2wt% of described melon colloidal suspension liquid gross weight;
3) stir and be warming up to 30-40 ℃;
4) add alkali lye and alkalization;
5) after alkalization finished, the dropping mol ratio was ampholytic ion pair monomer and the etherifying agent of 0.1-1: 1-0.1, and adds described alkali lye again;
6) be warming up to 50 ℃-70 ℃, reacted 4-6 hour;
7) after reaction finished, washing, drying, pulverizing were promptly;
Wherein said zwitter-ion is to being:
R wherein
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical COO
-Or sulfonate radical SO
3 -Wherein etherifying agent is selected from propylene oxide, chloroethanol, sodium chloroacetate and 3-chloro-2-hydroxypropyl-N, N, N-trimethyl ammonium chloride; Wherein alkali lye is the aqueous solution of sodium hydroxide or yellow soda ash; With
B. prepared thickening material is mixed according to described amount with clay stabilizer, sterilant, cleanup additive and promptly get fracturing liquid.
5. method as claimed in claim 4, wherein said phase-transfer catalyst are selected from palmityl trimethyl ammonium chloride, 16 octadecyl trimethyl ammonium chloride and 14 palmityl trimethyl ammonium chlorides; Wherein solvent is selected from the mixing solutions of methyl alcohol, ethanol, propyl alcohol and water, and preferred volume ratio is the mixing solutions of 4: 1 second alcohol and water.
6. one kind prepares as claim 2 or 3 described of the fracturing fluid methods, and it comprises the steps:
A. at first prepare thickening material;
1) pre-treatment melon collagen powder;
2) be 2-3 with weight ratio: 1 solvent mix with pretreated melon collagen powder melon colloidal suspension liquid; The phase-transfer catalyst that adds the 0.01wt%-2wt% of described melon suspension;
3) stir and be warming up to 30-40 ℃;
4) add alkali lye and alkalization;
5) after alkalization finished, the dropping mol ratio was ampholytic ion pair monomer and the etherifying agent of 0.1-1: 1-0.1, and adds described alkali lye again;
6) be warming up to 50 ℃-70 ℃, reacted 4-6 hour;
7) after reaction finished, washing, drying, pulverizing were promptly;
Wherein zwitter-ion is to being:
R wherein
1And R
2Represent C respectively
1-C
4Alkyl, R
3Expression carboxylate radical COO
-Or sulfonate radical SO
3 -Wherein etherifying agent is selected from propylene oxide, chloroethanol, sodium chloroacetate and 3-chloro-2-hydroxypropyl-N, N, N-trimethyl ammonium chloride; Wherein alkali lye is the aqueous solution of sodium hydroxide or yellow soda ash; With
B. according to described amount with thickening material mix with clay stabilizer, sterilant, cleanup additive base fluid, and then add linking agent and carry out crosslinking reaction and promptly get fracturing liquid.
7. method as claimed in claim 6, wherein said phase-transfer catalyst are selected from palmityl trimethyl ammonium chloride, 16 octadecyl trimethyl ammonium chloride and 14 palmityl trimethyl ammonium chlorides; Wherein said solvent is selected from the mixing solutions of methyl alcohol, ethanol, propyl alcohol and water.
8. method as claimed in claim 6, wherein said solvent are that volume ratio is the mixing solutions of 4: 1 second alcohol and water.
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Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: China Oilfield Services Limited Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: China Oilfield Services Limited Patentee before: China National Offshore Oil Corporation |