CN104558404A - Hydrophobically associating polymer for shale gas exploitation - Google Patents
Hydrophobically associating polymer for shale gas exploitation Download PDFInfo
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Abstract
The invention relates to a hydrophobically associating polymer for shale gas exploitation and a preparation method thereof and an application of the hydrophobically associating polymer as a drag reducer in shale gas exploitation and is mainly used for solving the problem of low drag reduction rate of the polymers in the prior art. The hydrophobically associating polymer for shale gas exploitation is prepared from the following mixtures in parts by mass through free radical polymerization: a) 100 parts of acrylamide; b) 0-60 parts of free radical polymerization anion monomer; c) 0.1-60 parts of free radical polymerization hydrophobic monomer; and d) 200-2,000 parts of water; and the technical problem is solved relatively well by the technical scheme, and the hydrophobically associating polymer can be used as a drag reducer in shale gas exploitation.
Description
Technical field
The present invention relates to hydrophobic associated polymer, its preparation method for shale gas exploitation, and described hydrophobic associated polymer in shale gas exploitation as the application of flow improver.
Background technology
Along with hydrocarbon resources is increasingly in short supply, energy security problem becomes increasingly conspicuous, and shale gas resource has become the focus that countries in the world energy circle falls over each other to study.At present, Chinese shale gas resources exploration is still in explores the starting stage, and it is important topics that China's energy industry faces that exploitation protects these resources.Current shale gas exploitation uses hydraulic fracturing technology usually, because liquid displacement during shale gas pressure break is very large, need in clear water, to add a certain amount of flow improver as hydroxypropyl guar gum, polyacrylamide etc., be used for reducing the frictional resistance of liquid in pipeline, improve construction effect.But the polymer-based carbon pressure break system of routine is due to containing water-insoluble and colloid residue, easily cause the grievous injury of shale reservoir, fracturing liquid is unfavorable for the formation of stitching net after being cross-linked to form frozen glue, and can be increased in the frictional resistance in pipeline, therefore brings restriction to preparation of construction.The external transformation to shale oil gas reservoir at present, main employing slippery water system.In order to increase solvability and dispersing property, being usually made into by flow improver with mineral oil is the suspension of foreign minister, and the use of mineral oil considerably increases the difficulty returning discharge opeing process.Conventional hydroxypropyl guar gum is a kind of polygalactomannan, is easily degraded by microorganisms, therefore usually also needs to add a certain amount of sterilant in slippery water.The use of sterilant, brings more serious environmental problem, makes the process returning discharge opeing more complicated.Therefore, need to develop a kind of environment-friendly high-efficiency flow improver economic again, thus reduce operation pressure, improve construction technology success ratio and economic benefit.
Domesticly in the development of shale gas flow improver, be also in the starting stage, Southwest Petrol University, Sweet natural gas limited-liability company of PetroChina Company Limited., petroleum engineering Institute for Research and Technology of Henan Oil Field branch office of PetroChina Company Limited., northwest oilfield branch engineering and technological research institute of PetroChina Company Limited., extend the mechanisms such as oil in shale gas flow improver, all carried out research work, make some progress.
Publication number is the preparation method that patent reports a kind of shale gas flow improver of CN102977877A, and by introducing the method for function monomer on the polyacrylamide of routine, improve the anti-shear performance of flow improver, resistance-reducing yield can reach 70%; Publication number is the preparation method that the patent of CN102516975, CN103045226A and CN103010488A all reports smooth water type flow improver, but such flow improver resistance-reducing yield is all lower.
Summary of the invention
One of technical problem to be solved by this invention is the problem that the polymkeric substance resistance-reducing yield of prior art is low, and provide a kind of hydrophobic associated polymer for shale gas exploitation, this hydrophobic associated polymer has the high advantage of resistance-reducing yield.
Two of technical problem to be solved by this invention is preparation methods of the described hydrophobic associated polymer of one of above-mentioned technical problem.
Three of technical problem to be solved by this invention be the described hydrophobic associated polymer of one of above-mentioned technical problem in shale gas exploitation as the application of flow improver.
In order to one of solve the problems of the technologies described above, technical scheme of the present invention is as follows: for the hydrophobic associated polymer of shale gas exploitation, the mixture represented by following masses part obtains through radical polymerization:
A) acrylamide of 100 parts;
B) the radical polymerization anionic monomer of 0 ~ 60 part;
C) the radical polymerization hydrophobic monomer of 0.1 ~ 60 part;
D) water of 200 ~ 2000 parts.
In technique scheme, at least one of described radical polymerization anionic monomer preferably in 2-acrylamide-2-methylpro panesulfonic acid, vinylformic acid, methacrylic acid, vinylbenzenesulfonic acid, vinyl sulfonic acid.
In technique scheme, the one of described radical polymerization hydrophobic monomer preferably in negatively charged ion hydrophobic monomer or cation hydrophobic monomer; Described negatively charged ion hydrophobic monomer has the general formula shown in formula (I); Described cation hydrophobic monomer has the general formula shown in formula (II); R
1c
4~ C
16alkyl, M is selected from NH
4or any one in basic metal; R
3and R
4independently be selected from C
1~ C
4alkyl, R
2for C
12~ C
22alkyl, X is halogen, and X is chlorine more preferably;
（I）；
（II）。
As most preferred technical scheme, described hydrophobic associated polymer, the mixture represented by following masses part obtains through radical polymerization:
A) acrylamide of 100 parts;
B) the 2-acrylamide-2-methylpro panesulfonic acid of 50 ~ 60 parts;
C) the negatively charged ion hydrophobic monomer shown in formula (I) of 0.1 ~ 2 part, wherein R
1for C
8~ C
12alkyl, M is selected from NH
4or any one in basic metal;
D) water of 500 ~ 700 parts.
In above-mentioned most preferred technical scheme, the most preferably R
1for C
10alkyl.
For solve the problems of the technologies described above two, technical scheme of the present invention is as follows: the preparation method of the hydrophobic associated polymer described in the technical scheme of one of above-mentioned technical problem, comprises following step successively:
A () adds water, acrylamide, radical polymerization anionic monomer, radical polymerization hydrophobic monomer in polymeric kettle, stir formation solution;
B pH value to 7 ~ 10 of () regulator solution, add radical polymerization initiator, cause 0.5 ~ 1 hour the temperature of 10 ~ 30 DEG C;
C () is polymerized 2 ~ 8 hours at the temperature of 40 ~ 60 DEG C, obtain moisture gel hydrophobic associated polymer.
In technique scheme, described radical initiator is preferably redox initiator.
In technique scheme, described radical initiator consumption preferably accounts for 0.003 ~ 0.5% of described total weight of monomer.
In technique scheme, described radical initiator preferably forms by being selected from least one oxygenant and at least one reductive agent be selected from alkali metal sulfite, alkali metal bisulfite or alkali metal thiosulfate in ammonium persulphate or alkali metal persulphate.
In technique scheme, preferably also comprise the steps: after described step (c)
D () is dry, obtain the hydrophobic associated polymer of dry state.
In technique scheme, the temperature of described step (d) drying is preferably 80 ~ 95 DEG C.
For solve the problems of the technologies described above three, technical scheme of the present invention is as follows: the described hydrophobic associated polymer of one of above-mentioned technical problem in shale gas exploitation as the application of flow improver.
The drag reduction aqueous solution huge discharge that described hydrophobic associated polymer is preferably made into 0.005 ~ 0.2wt% by the such as method of described application injects bottom fast, effectively can reduce the circulation friction pressure in operation.
Key problem in technology of the present invention have employed hydrophobic monomer in acrylamide copolymer, when flow improver concentration of the present invention is 0.005 ~ 0.2wt%, resistance-reducing yield can reach more than 76%, do not adopt the acrylamide copolymer resistance-reducing yield of hydrophobic monomer to be only 60%, achieve good technique effect.
Embodiment
[embodiment 1]
1, the synthesis of polymkeric substance
In polymeric kettle, first add 650g deionized water, add 100g acrylamide (AM), 54g 2-acrylamide-2-methylpro panesulfonic acid (AMPS), 1.5g 2-acrylamido sodium laurylsulfonate (NaAMC
12s), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, the persulfate aqueous solution 15.5g of the aqueous solution of sodium bisulfite 15.5g and 0. 1wt% that then add 0.1wt% successively, as initiator, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain moisture gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain the hydrophobic associated polymer of dry state.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Except flow improver solution with 10L/min traffic flow except 1/2 inch of pipe, other carries out the indoor resistance-reducing performance evaluation of friction-reducing agent of fracturing fluid according to the method for 7.13.1 in SY/T 6376-2008 fracturing liquid general technical specifications.Clear water is loaded Multifunctional flowing loop instrument, measure clear water by stable pressure differential deltap during pipeline
p 1; Measure stable pressure differential deltap when above-mentioned friction-reducing agent of fracturing fluid flows through pipeline after the same method
p 2, calculate resistance-reducing yield η by formula (1):
（1）
The results are shown in subordinate list 1.
Present inventor finds, when described hydrophobic associated polymer, when the mixture represented by following masses part obtains through radical polymerization, resistance reducing effect is best: a) acrylamide of 100 parts; B) the 2-acrylamide-2-methylpro panesulfonic acid of 50 ~ 60 parts; C) the negatively charged ion hydrophobic monomer shown in formula (I) of 0.1 ~ 2 part, wherein R
1for C
8~ C
12alkyl, M is selected from NH
4or any one in basic metal; D) water of 500 ~ 700 parts.This also can from embodiment 1 and other embodiment and comparative example on year-on-year basis intuitively find out.
[embodiment 2]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 60g2-acrylamide-2-methylpro panesulfonic acid (AMPS), 15g 2-acrylamido sodium laurylsulfonate (NaAMC
12s), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, persulfate aqueous solution 17.5 g of the aqueous solution of sodium bisulfite 17.5g and 0. 1wt% that then add 0. 1wt% successively, as initiator, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobically associating polymers.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[embodiment 3]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 55.5g2-acrylamido sodium laurylsulfonate (NaAMC
12s), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, the persulfate aqueous solution 10g of the aqueous solution of sodium bisulfite 10g and 0. 1wt% that then add 0.1wt% successively, as initiator, seals after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobically associating polymers, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[
embodiment 4]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 40g methacrylic acid (MAA), 12g solution property (C
18dMAA), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then add the persulfate aqueous solution 15.2g of aqueous solution of sodium bisulfite 15.2g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobically associating polymers, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[embodiment 5]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 30g vinylformic acid (AA), 9g hexadecyldimethyl benzyl ammonium allyl ammonium chloride (C
16dMAA), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then add the persulfate aqueous solution 13.9g of aqueous solution of sodium bisulfite 13.9g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[embodiment 6]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 20g vinylbenzenesulfonic acid (VBS), 6g2-acrylamido tetradecyl sodium sulfonate (NaAMC
14s) be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then add the persulfate aqueous solution 12.3g of aqueous solution of sodium bisulfite 12.3g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[embodiment 7]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 10g vinylformic acid (AA), 3g 2-acrylamido ten alkyl sodium sulfonate (NaAMC
10s), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then add the persulfate aqueous solution 11.3g of aqueous solution of sodium bisulfite 11.3g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[embodiment 8]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 5g2-acrylamide-2-methylpro panesulfonic acid (AMPS), 1g 2-acrylamido octyl sodium sulfonate (NaAMC
8s), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then add the persulfate aqueous solution 10.6g of aqueous solution of sodium bisulfite 10.6g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain hydrophobic associated polymer.
2, the preparation of flow improver
In 10L water, add 1g hydrophobic associated polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
[
comparative example]
1, the synthesis of polymkeric substance
First add 650g deionized water in a kettle., add 100g acrylamide (AM), 55.5g 2-acrylamide-2-methylpro panesulfonic acid (AMPS), be stirred to and dissolve completely, be 9 by NaOH adjust ph, and start to pass into high pure nitrogen, after 30min, temperature in the kettle is down to 15 DEG C, then adds the persulfate aqueous solution 15.4g of aqueous solution of sodium bisulfite 15.4g and 0.1wt% of 0.1wt% successively as initiator, seal after continuing logical nitrogen 30min.After 1 hour, temperature of reaction is risen to 45 DEG C gradually, react and obtain gel polymerisate after 3 hours, to cut after glue forced air drying 1.5h under 90 oC, smash to sieve with pulverizer and obtain acrylamide copolymerized polymer.
2, the preparation of flow improver
In 10L water, add 1g acrylamide copolymerized polymer, stir 20 minutes under the speed of mechanical stirring 200rpm, obtain the flow improver solution of 0.01wt%.
3, the performance test of flow improver
Testing method is identical with embodiment 1, the results are shown in subordinate list 1.
Present inventor finds, in raising resistance-reducing yield, and negatively charged ion hydrophobic monomer (the wherein R shown in AMPS and formula (I)
1for C
8~ C
12alkyl, M is selected from NH
4or any one in basic metal) there is synergy.From comparative example, embodiment 1 and embodiment 3 on year-on-year basis also can visually see.
Table 1 embodiment and comparative example resistance-reducing yield result
Claims (10)
1., for the hydrophobic associated polymer of shale gas exploitation, the mixture represented by following masses part obtains through radical polymerization:
A) acrylamide of 100 parts;
B) the radical polymerization anionic monomer of 0 ~ 60 part;
C) the radical polymerization hydrophobic monomer of 0.1 ~ 60 part;
D) water of 200 ~ 2000 parts.
2. hydrophobic associated polymer according to claim 1, is characterized in that described radical polymerization anionic monomer is selected from least one in 2-acrylamide-2-methylpro panesulfonic acid, vinylformic acid, methacrylic acid, vinylbenzenesulfonic acid, vinyl sulfonic acid.
3. hydrophobic associated polymer according to claim 1, is characterized in that described radical polymerization hydrophobic monomer is selected from the one in negatively charged ion hydrophobic monomer or cation hydrophobic monomer; Described negatively charged ion hydrophobic monomer has the general formula shown in formula (I); Cation hydrophobic monomer has the general formula shown in formula (II); R
1c
4~ C
16alkyl, M is selected from NH
4or any one in basic metal; R
3and R
4independently be selected from C
1~ C
4alkyl, R
2for C
12~ C
22alkyl, X is halogen;
（I）；
（II）。
4. the preparation method of hydrophobic associated polymer according to claim 1, comprises following step successively:
A () adds water, acrylamide, radical polymerization anionic monomer, radical polymerization hydrophobic monomer in polymeric kettle, stir formation solution;
B pH value to 7 ~ 10 of () regulator solution, add radical polymerization initiator, cause 0.5 ~ 1 hour the temperature of 10 ~ 30 DEG C;
C () is polymerized 2 ~ 8 hours at the temperature of 40 ~ 60 DEG C, obtain moisture gel hydrophobic associated polymer.
5. the preparation method of hydrophobic associated polymer according to claim 4, is characterized in that described radical initiator is redox initiator.
6. the preparation method of hydrophobic associated polymer according to claim 4, is characterized in that described radical initiator consumption is account for described total weight of monomer 0.003 ~ 0.5%.
7. the preparation method of hydrophobic associated polymer according to claim 5, is characterized in that described radical initiator forms by being selected from least one oxygenant and at least one reductive agent be selected from alkali metal sulfite, alkali metal bisulfite or alkali metal thiosulfate in ammonium persulphate or alkali metal persulphate.
8. the preparation method of hydrophobic associated polymer according to claim 4, also comprises the steps: after it is characterized in that step (c)
D () is dry, obtain the hydrophobic associated polymer of dry state.
9. the preparation method of hydrophobic associated polymer according to claim 5, is characterized in that the temperature of step (d) drying is 80 ~ 95 DEG C.
10. the hydrophobic associated polymer described in claim 1 in shale gas exploitation as the application of flow improver.
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Cited By (5)
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| CN106967196A (en) * | 2017-02-27 | 2017-07-21 | 西南石油大学 | A kind of high temperature resistant PAMC inhibitor and its preparation method and application |
| CN108250357A (en) * | 2018-01-26 | 2018-07-06 | 重庆科技学院 | A kind of method that no soap method prepares cation-type hydrophobic association type polyacrylamide |
| CN109135714A (en) * | 2018-09-17 | 2019-01-04 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of long-acting antiseptic resistance-reducing agent |
| CN112778455A (en) * | 2020-12-30 | 2021-05-11 | 宁波锋成先进能源材料研究院有限公司 | Temperature-resistant salt-resistant hydrophobic association polymer and preparation method and application thereof |
| CN113214816A (en) * | 2021-05-14 | 2021-08-06 | 西南石油大学 | Variable-viscosity slippery water and preparation method thereof |
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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 |
| CN103333672A (en) * | 2013-01-11 | 2013-10-02 | 中国石油天然气股份有限公司 | Salt-tolerant resistance-reducing agent applied for shale gas reservoir |
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| US20030022987A1 (en) * | 1999-07-16 | 2003-01-30 | Matz Gary F. | Water soluble polymer composition and method of use |
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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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| CN106967196A (en) * | 2017-02-27 | 2017-07-21 | 西南石油大学 | A kind of high temperature resistant PAMC inhibitor and its preparation method and application |
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| CN112778455A (en) * | 2020-12-30 | 2021-05-11 | 宁波锋成先进能源材料研究院有限公司 | Temperature-resistant salt-resistant hydrophobic association polymer and preparation method and application thereof |
| CN113214816A (en) * | 2021-05-14 | 2021-08-06 | 西南石油大学 | Variable-viscosity slippery water and preparation method thereof |
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| CN104558404B (en) | 2017-01-25 |
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