CN105647506A - Clay stabilizer used for oil and gas field fracturing and preparation method thereof - Google Patents
Clay stabilizer used for oil and gas field fracturing and preparation method thereof Download PDFInfo
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- 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
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
- C08G65/2624—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aliphatic amine groups
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
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- 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
- C09K8/607—Compositions for stimulating production by acting on the underground formation specially adapted for clay formations
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- 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
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- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/50—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing nitrogen, e.g. polyetheramines or Jeffamines(r)
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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Abstract
The invention discloses a clay stabilizer used for oil and gas field fracturing and a preparation method thereof and belongs to the technical field of oil and gas filed exploitation. With polyethylene polyamine being an initiator, the initiator and ethylene oxide and/or propylene oxide are subjected to a ring opening addition reaction, and then an amine cationization reaction is performed to prepare the clay stabilizer which can effectively prevent clay and clay shale from expanding. Compatibility between the clay stabilizer and all kinds of water-soluble polymer thickening agents, particularly an artificially synthesized polyacrylamide macromolecule drag-reduction agent is good, and the clay stabilizer is suitable for being used for drag-reduction water fracturing fluid of oil and gas field large-scale volume fracturing, wherein the structural general formula of the clay stabilizer is displayed as follows.
Description
Technical field
The present invention relates to a kind of oil-gas field fracturing clay stabilizer, the preparation method also relating to this clay stabilizer, belong to exploitation of oil-gas field technical field.
Background technology
Oil gas field reservoir all contains a certain amount of clay mineral (such as Kaolin, montmorillonite, illite, chlorite, illite/smectite mixed layer etc.), when reservoir being carried out water-based fracturing transformation, clay can expand, migrate, very easily blocking duct, stratum and pore structure throat, reduce in-place permeability, thus causing the oil well underproduction.
For reducing the hydration swelling of clay mineral, expansion-resisting agent must be added in fracturing fluid with stable clay. At present, oil field at home for hyposmosis, water-sensitive oil-gas Layer frequently with Cationic Polymers Containing Quaternary Ammonium Salts, as polyepichlorohydrin-dimethylamine, poly-trimethylallylammonium chloride, PDDA and acrylamide, dimethyl diallyl ammonium chloride, acrylyl oxy-ethyl-trimethyl salmiac copolymer etc. But, Cationic Polymers Containing Quaternary Ammonium Salts contains substantial amounts of cationic species, after contacting with anionic additive, owing to there is electrostatic adsorption between zwitterion, easily reduce of the fracturing fluid compatibility and preventive effect of expansion, serious even appearance is muddy, flocculation and delamination phenomenon, greatly limit its application.
The patent of invention of publication No. CN102433110A discloses a kind of amine shale stabilizer for drilling fluid, polyether diamine react generation with epoxyalkane according to mol ratio 10:1��1:20, and its structural formula is as follows:
In formula 1: R, R ' alkylidene of respectively carbon number 2��4, m, n take any integer in 0��10 respectively. Preferably, polyether diamine is polyethyleneoxide diamine, polypropyleneoxide diamine or polyoxyethylenepropylene diamidogen, and molecular weight is hydrogen or methyl less than 1000, R, 1��x+y+z��20. This stabilizer can effectively suppress hydration and expansion of clay and aquation dispersion, but its compatibility is poor, and anti-swollen performance need further raising.
Summary of the invention
It is an object of the invention to provide a kind of oil-gas field fracturing clay stabilizer, its anti-swollen excellent performance, compatibility is good.
Meanwhile, the preparation method that the present invention also provides for a kind of above-mentioned clay stabilizer.
In order to realize object above, the technical solution adopted in the present invention is:
Oil-gas field fracturing clay stabilizer, its general structure is as follows:
In formula 2: A is polyoxyethylene groups (EO), B is polyoxypropylene base (PO), and x, y take any integer in 0��10 respectively, and z takes any integer in 2��10; R is hydrogen, the alkyl of 1��5 carbon, the hydroxyalkyl of 1��5 carbon or-CH2-COONa; N takes any integer in 0��5.
Preferably, in formula 2, x takes any integer in 0��6, and y takes any integer in 0��4, and z takes any integer in 2��5, and R is hydrogen, methyl or-CH2-COONa��
It is further preferred that in formula 2, x takes 0, y and takes 0 or 3, z to take 4 or 5, R be hydrogen or methyl.
More excellent, in formula 2, x takes 0, y and takes 0 or 3, z to take 5, R be methyl.
Optimum, in formula 2, x takes 0, y and takes 3, z to take 5, R be methyl.
The preparation method of oil-gas field fracturing clay stabilizer, is with polyethylene polyamine for initiator, after oxirane and/or expoxy propane open loop addition, then carries out the positive ionization of amine.
The general structure of described polyethylene polyamine is as follows:
In formula 3: n takes any integer in 0��5.
The mol ratio of described polyethylene polyamine and oxirane and/or expoxy propane is 1:(n+4) �� (x+y+z).
The concrete operations of described cationoid reaction are: add solvent and cationic reagent in open loop addition products therefrom, react 0.5��15h at temperature 25��100 DEG C. Wherein, cationic reagent can be selected for the halogenated carboxylic acid salt (such as sodium chloroacetate) of formic acid, acetic acid, phosphoric acid, citric acid, the alkyl halide (such as chloromethanes, ethyl chloride) of 1��5 carbon, the halohydrin (such as 2-chloroethyl alcohol) of 1��5 carbon or 2��5 carbon. Solvent can be selected for the aqueous solution of ethanol, isopropanol or ethylene glycol, and the concentration of alcoholic solution is 20%��80%; The addition of solvent is the 20%��70% of opening product (polyethylene polyamine polyethers) quality, namely is made into the polyethylene polyamine polyether solutions of concentration 58.8%��80%. Adding solvent can make positive ionization be smoothed out on the one hand, can control the freezing point of final products on the other hand, meet low temperature instructions for use. The pH value of gained clay stabilizer is 7��9.
Beneficial effects of the present invention:
In the present invention, oil-gas field fracturing clay stabilizer is with polyethylene polyamine for initiator, after oxirane and/or expoxy propane open loop addition, the positive ionization carrying out amine again prepares, this clay stabilizer can effectively prevent clay, mud shale expansion, with various water soluble polymer thickening agents, especially synthetic polyacrylamide polymer drag reducing agent has good compatibility, suitable in the fracturing reform of hyposmosis densification oil shale and sensitive reservoir, it is adapted in oil gas field extensive volume fracturing drag reduction water fracturing fluid and uses.
Detailed description of the invention
The present invention is only described in further detail by following embodiment, but does not constitute any limitation of the invention.
Embodiment 1
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) triethylene tetramine 146g (1mol) and catalyst potassium hydroxide 1.5g is joined in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to oxirane 1584g (36mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, be cooled to room temperature, obtain faint yellow liquid product;
2) weigh above-mentioned product 173g, add dehydrated alcohol 50g and water 200g, drip acetic acid 20g, obtain transparent clay stabilizer.
Embodiment 2
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) TEPA 189g (1mol) and catalyst potassium hydroxide 2.0g is joined in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to oxirane 1232g (28mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, be cooled to room temperature, obtain faint yellow liquid product;
2) weighing above-mentioned product 142g, add dehydrated alcohol 50g and water 200g, drip sodium chloroacetate 55g, be warming up to 80 DEG C of back flow reaction 8h, cooling obtains transparent clay stabilizer.
Embodiment 3
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) polyethylene polyamine 253.5g (five hexamine, the six ethylene seven each 0.5mol of amine) and catalyst potassium hydroxide 2.5g is joined in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to oxirane 1870g (42.5mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, be cooled to room temperature, obtain faint yellow liquid product;
2) weighing above-mentioned product 142g, add dehydrated alcohol 50g and water 200g, drip chloromethanes 52.8g, be warming up to 60 DEG C of back flow reaction 3h, cooling obtains transparent clay stabilizer.
Embodiment 4
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) by polyethylene polyamine 253.5g (five hexamine, the six ethylene seven each 0.5mol of amine) and catalyst potassium hydroxide 2.5g join in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to expoxy propane 1479g (25.5mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, it is slow added into oxirane 1496g (34mol), control reaction temperature 140 �� 5 DEG C, react complete, it is cooled to room temperature, obtain faint yellow liquid product,
2) weigh above-mentioned product 323g, add dehydrated alcohol 100g and water 300g, drip formic acid 28g, obtain transparent clay stabilizer.
Embodiment 5
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) by polyethylene polyamine 253.5g (five hexamine, the six ethylene seven each 0.5mol of amine) and catalyst potassium hydroxide 2.5g join in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to expoxy propane 1479g (25.5mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, it is slow added into oxirane 1870g (42.5mol), control reaction temperature 140 �� 5 DEG C, react complete, it is cooled to room temperature, obtain faint yellow liquid product,
2) weighing above-mentioned product 362g, add dehydrated alcohol 100g and water 300g, drip chloromethanes 52.8g, be warming up to 60 DEG C of back flow reaction 3h, cooling obtains transparent clay stabilizer.
Embodiment 6
In the present embodiment, the structural formula of oil-gas field fracturing clay stabilizer is as follows:
Its preparation process includes:
1) by polyethylene polyamine 253.5g (five hexamine, the six ethylene seven each 0.5mol of amine) and catalyst potassium hydroxide 2.5g join in autoclave, when being warming up to 100 �� 5 DEG C, gauge pressure is pumped it to for-0.08MPa with vacuum pump, with nitrogen sparge tube road and reactor 2 times, stir and heat up, when temperature rises to 130 �� 5 DEG C, it is slowly added to oxirane 1496g (34mol), control reaction temperature 140 �� 5 DEG C, charging rate is to maintain gauge pressure 0.25 �� 0.05MPa, react complete, it is slowly added to expoxy propane 1479g (25.5mol), control reaction temperature 140 �� 5 DEG C, react complete, it is slow added into oxirane 1496g (34mol), control reaction temperature 140 �� 5 DEG C, react complete, it is cooled to room temperature, obtain faint yellow liquid product,
2) weighing above-mentioned product 472g, add isopropanol 300g and water 450g, drip sodium chloroacetate 99g, be warming up to 60 DEG C of back flow reaction 3h, cooling obtains transparent clay stabilizer.
Test example
1, anti-swollen performance test
The clay stabilizer of Example 1��6 preparation, anti-dilative is measured according to People's Republic of China's oil and gas industry standard SY/T5971-94 water filling clay stabilizer method of evaluating performance, requiring to measure water-fastness rate according to China PetroChemical Corporation standard Q/SH0053-2010 clay stabilizer technology, result is shown in table 1 below.
The anti-swollen the performance test results of clay stabilizer in table 1 embodiment 1��6
As shown in Table 1, in embodiment 1��6, clay stabilizer has the anti-swollen performance of excellence.
2, compatibility test
The clay stabilizer of Example 1��6 preparation, composite with commercially available thickening agent (0.3% thickening agent+1% clay stabilizer, surplus is water), investigate its compatibility, result is shown in table 2 below.
The compatibility evaluation result of clay stabilizer and commercially available thickening agent in table 2 embodiment 1��6
As shown in Table 2, without floccule or flocculation phenomenon appearance after clay stabilizer and non-ionic hydroxypropyl guar gum in embodiment 1��6, anion-polyacrylamide, cationic-type polyacrylamide class thickening agent are composite, compatibility is good.
Claims (10)
1. oil-gas field fracturing clay stabilizer, it is characterised in that: the general structure of described clay stabilizer is as follows:
In formula 2: A is polyoxyethylene groups, B is polyoxypropylene base, and x, y take any integer in 0��10 respectively, and z takes any integer in 2��10; R is hydrogen, the alkyl of 1��5 carbon, the hydroxyalkyl of 1��5 carbon or-CH2-COONa; N takes any integer in 0��5.
2. clay stabilizer according to claim 1, it is characterised in that: in formula 2, x takes any integer in 0��6, and y takes any integer in 0��4, and z takes any integer in 2��5, and R is hydrogen, methyl or-CH2-COONa��
3. clay stabilizer according to claim 2, it is characterised in that: in formula 2, x takes 0, y and takes 0 or 3, z to take 4 or 5, R be hydrogen or methyl.
4. clay stabilizer according to claim 3, it is characterised in that: in formula 2, x takes 0, y and takes 0 or 3, z to take 5, R be methyl.
5. the preparation method of clay stabilizer as according to any one of Claims 1 to 4, it is characterised in that: with polyethylene polyamine for initiator, after oxirane and/or expoxy propane open loop addition, then carry out the positive ionization of amine.
6. preparation method according to claim 5, it is characterised in that: the general structure of described polyethylene polyamine is as follows:
In formula 3: n takes any integer in 0��5.
7. preparation method according to claim 6, it is characterised in that: the mol ratio of described polyethylene polyamine and oxirane and/or expoxy propane is 1:(n+4) �� (x+y+z).
8. preparation method according to claim 7, it is characterised in that: described cationoid reaction is: add solvent and cationic reagent in open loop addition products therefrom, reacts 0��15h at temperature 0��100 DEG C.
9. preparation method according to claim 8, it is characterised in that: described cationic reagent is the halogenated carboxylic acid salt of formic acid, acetic acid, phosphoric acid, citric acid, the alkyl halide of 1��5 carbon, the halohydrin of 1��5 carbon or 2��5 carbon.
10. preparation method according to claim 8, it is characterised in that: described solvent is the aqueous solution of ethanol, isopropanol or ethylene glycol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329902A (en) * | 2018-01-23 | 2018-07-27 | 中国石油天然气股份有限公司 | A kind of salt tolerant clay stabilizer and preparation method thereof of oil field water outlet preparing fracturing fluid |
| CN110268034A (en) * | 2016-12-09 | 2019-09-20 | 赢创德固赛有限公司 | Shale hydration inhibitor |
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| CN104556771A (en) * | 2014-10-11 | 2015-04-29 | 江苏苏博特新材料股份有限公司 | Clay inhibitor as well as preparation method and application thereof |
| CN104559958A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Compound type polyamine shale inhibitor and preparation method thereof |
| CN104592955A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司 | Polyamine shale inhibitor and preparation method thereof |
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| CN104559958A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Compound type polyamine shale inhibitor and preparation method thereof |
| CN104592955A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司 | Polyamine shale inhibitor and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110268034A (en) * | 2016-12-09 | 2019-09-20 | 赢创德固赛有限公司 | Shale hydration inhibitor |
| CN110268034B (en) * | 2016-12-09 | 2022-09-06 | 赢创运营有限公司 | Shale hydration inhibition agent |
| CN108329902A (en) * | 2018-01-23 | 2018-07-27 | 中国石油天然气股份有限公司 | A kind of salt tolerant clay stabilizer and preparation method thereof of oil field water outlet preparing fracturing fluid |
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