CN105647506B - Oil-gas field fracturing clay stabilizer and preparation method thereof - Google Patents
Oil-gas field fracturing clay stabilizer and preparation method thereof Download PDFInfo
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
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- C08G65/2624—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
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Abstract
The invention discloses a kind of oil-gas field fracturing clay stabilizers and preparation method thereof, belong to exploitation of oil-gas field technical field.The clay stabilizer is using polyethylene polyamine as initiator, after ethylene oxide and/or propylene oxide open loop addition, the positive ionization for carrying out amine again is made, it can effectively prevent clay, mud shale expansion, with various water soluble polymer thickeners, there is especially artificial synthesized polyacrylamide polymer drag reducing agent good compatibility to be suitble to use in the extensive volume fracturing drag reduction water fracturing fluid of oil gas field suitable for hyposmosis densification oil shale and the fracturing reform of sensitive reservoir.The general structure of clay stabilizer is as follows:
Description
Technical field
The present invention relates to a kind of oil-gas field fracturing clay stabilizers, also relate to the preparation side of the clay stabilizer
Method belongs to exploitation of oil-gas field technical field.
Background technique
Oil gas field reservoir contains a certain amount of clay mineral, and (such as kaolin, montmorillonite, illite, chlorite, she deceives people
Layer etc.), when carrying out water-based fracturing transformation to reservoir, clay can expand, migrate, easily blocking stratum duct and pore structure larynx
Portion reduces in-place permeability, so as to cause the oil well underproduction.
For the hydration swelling for reducing clay mineral, expansion-resisting agent must be added in fracturing fluid to stablize clay.Currently, domestic oil
Field is directed to hyposmosis, water-sensitive oil-gas Layer frequently with Cationic Polymers Containing Quaternary Ammonium Salts, such as polyepichlorohydrin-dimethylamine, poly- three
Methacrylic chlorination ammonium, polydimethyl diallyl ammonium chloride and acrylamide, dimethyl diallyl ammonium chloride, propylene
The copolymer etc. of acyloxyethyl trimethyl ammonium chloride.But Cationic Polymers Containing Quaternary Ammonium Salts contain a large amount of cationic species,
After contacting with anionic additive, since there are electrostatic adsorptions between zwitterion, the compatibility of fracturing fluid is easily reduced
And preventive effect of expansion, serious or even appearance muddiness, 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, by polyethers
Diamines reacts generation according to molar ratio 10:1~1:20 with epoxyalkane, and structural formula is as follows:
In formula 1: R, R ' be respectively carbon atom number 2~4 alkylidene, m, n take any integer in 0~10 respectively.Preferably,
Polyether diamine be polyethyleneoxide diamine, polypropyleneoxide diamine or polyoxyethylenepropylene diamines, molecular weight less than 1000, R be hydrogen or
Methyl, 1≤x+y+z≤20.The stabilizer can effectively inhibit hydration and expansion of clay and aquation to disperse, but its compatibility is poor, prevent
It still needs further improvement for swollen performance.
Summary of the invention
The object of the present invention is to provide a kind of oil-gas field fracturing clay stabilizer, prevent it is swollen have excellent performance, compatibility is good
It is good.
Meanwhile the present invention also provides a kind of preparation methods of above-mentioned clay stabilizer.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
Oil-gas field fracturing clay stabilizer, general structure are as follows:
In formula 2: A is polyoxyethylene groups (EO), and B is polyoxypropylene base (PO), and x, y take any integer in 0~10, z respectively
Take any integer in 2~10；R is the hydroxyalkyl or-CH of hydrogen, the alkyl of 1~5 carbon, 1~5 carbon2-COONa；N takes 0~5
Middle any integer.
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, R
For hydrogen, methyl or-CH2-COONa。
It is further preferred that it is hydrogen or methyl that x, which takes 0, y that 0 or 3, z is taken to take 4 or 5, R, in formula 2.
More preferably, in formula 2, it is methyl that x, which takes 0, y that 0 or 3, z is taken to take 5, R,.
Optimal, in formula 2, it is methyl that x, which takes 0, y that 3, z is taken to take 5, R,.
The preparation method of oil-gas field fracturing clay stabilizer, be using polyethylene polyamine as initiator, with ethylene oxide and/
Or after propylene oxide open loop addition, then carry out the positive ionization of amine.
The general structure of the polyethylene polyamine is as follows:
In formula 3: n takes any integer in 0~5.
The molar ratio of the polyethylene polyamine and ethylene oxide and/or propylene oxide is 1:(n+4) × (x+y+z).
The concrete operations of the cationoid reaction are as follows: solvent and cationization examination are added in open loop addition products therefrom
0.5~15h is reacted in agent at 25~100 DEG C of temperature.Wherein, cationic reagent can be selected formic acid, acetic acid, phosphoric acid,
Citric acid, the alkyl halide (such as chloromethanes, chloroethanes) of 1~5 carbon, the halohydrin (such as chlorethanol) of 1~5 carbon or 2~5
The halogenated carboxylic acid salt (such as sodium chloroacetate) of carbon.Solvent can be selected the aqueous solution of ethyl alcohol, isopropanol or ethylene glycol, alcoholic solution it is dense
Degree is 20%~80%；The additional amount of solvent be opening product (polyethylene polyamine polyethers) quality 20%~
70%, namely it is made into the polyethylene polyamine polyether solutions of concentration 58.8%~80%.On the one hand solvent, which is added, can make to be cationized
Reaction is gone on smoothly, and on the other hand can control the freezing point of final products, meets low temperature requirement.Gained clay stabilizer
PH value is 7~9.
Beneficial effects of the present invention:
In the present invention oil-gas field fracturing with clay stabilizer be using polyethylene polyamine as initiator, with ethylene oxide and/or
After propylene oxide open loop addition, then carry out amine positive ionization be made, which can effectively prevent clay, mud page
Rock expansion, with various water soluble polymer thickeners, especially artificial synthesized polyacrylamide polymer drag reducing agent has good
Good compatibility is suitble to extensive in oil gas field suitable for hyposmosis densification oil shale and the fracturing reform of sensitive reservoir
It is used in volume fracturing drag reduction water fracturing fluid.
Specific embodiment
Only invention is further described in detail for following embodiments, but does not constitute any limitation of the invention.
Embodiment 1
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) triethylene tetramine 146g (1mol) and catalyst potassium hydroxide 1.5g are added in autoclave, are warming up to
At 100 ± 5 DEG C, gauge pressure is pumped it to vacuum pump and is stirred and is risen with nitrogen sparge tube road and reaction kettle 2 times for -0.08MPa
Temperature is slowly added to ethylene oxide 1584g (36mol) when temperature rises to 130 ± 5 DEG C, controls 140 ± 5 DEG C of reaction temperature, into
Speed is expected to maintain 0.25 ± 0.05MPa of gauge pressure, and end of reaction is cooled to room temperature, and obtains faint yellow liquid product；
2) above-mentioned product 173g is weighed, dehydrated alcohol 50g and water 200g is added, acetic acid 20g is added dropwise to get transparent clay
Stabilizer.
Embodiment 2
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) tetraethylenepentamine 189g (1mol) and catalyst potassium hydroxide 2.0g are added in autoclave, are warming up to
At 100 ± 5 DEG C, gauge pressure is pumped it to vacuum pump and is stirred and is risen with nitrogen sparge tube road and reaction kettle 2 times for -0.08MPa
Temperature is slowly added to ethylene oxide 1232g (28mol) when temperature rises to 130 ± 5 DEG C, controls 140 ± 5 DEG C of reaction temperature, into
Speed is expected to maintain 0.25 ± 0.05MPa of gauge pressure, and end of reaction is cooled to room temperature, and obtains faint yellow liquid product；
2) above-mentioned product 142g is weighed, dehydrated alcohol 50g and water 200g is added, sodium chloroacetate 55g is added dropwise, is warming up to 80 DEG C
Back flow reaction 8h, cooling obtain transparent clay stabilizer.
Embodiment 3
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) by polyethylene polyamine 253.5g (pentaethylene hexamine, each 0.5mol of six ethylene, seven amine) and catalyst potassium hydroxide
2.5g is added in autoclave, and when being warming up to 100 ± 5 DEG C, pumping it to gauge pressure with vacuum pump is -0.08MPa, uses nitrogen
Scavenging pipeline and reaction kettle 2 times, stir and heat up, when temperature rises to 130 ± 5 DEG C, be slowly added to ethylene oxide 1870g
(42.5mol) controls 140 ± 5 DEG C of reaction temperature, and for charging rate to maintain 0.25 ± 0.05MPa of gauge pressure, end of reaction is cooling
To room temperature, faint yellow liquid product is obtained；
2) above-mentioned product 142g is weighed, dehydrated alcohol 50g and water 200g is added, chloromethanes 52.8g is added dropwise, is warming up to 60 DEG C
Back flow reaction 3h, cooling obtain transparent clay stabilizer.
Embodiment 4
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) by polyethylene polyamine 253.5g (pentaethylene hexamine, each 0.5mol of six ethylene, seven amine) and catalyst potassium hydroxide
2.5g is added in autoclave, and when being warming up to 100 ± 5 DEG C, pumping it to gauge pressure with vacuum pump is -0.08MPa, uses nitrogen
Scavenging pipeline and reaction kettle 2 times, stir and heat up, when temperature rises to 130 ± 5 DEG C, be slowly added to propylene oxide 1479g
(25.5mol) controls 140 ± 5 DEG C of reaction temperature, and charging rate is to maintain 0.25 ± 0.05MPa of gauge pressure, end of reaction, then delays
It is slow that ethylene oxide 1496g (34mol) is added, 140 ± 5 DEG C of reaction temperature are controlled, end of reaction is cooled to room temperature, and is obtained yellowish
Color liquid product；
2) above-mentioned product 323g is weighed, dehydrated alcohol 100g and water 300g is added, formic acid 28g is added dropwise and is glued to get transparent
Soil stabilizer.
Embodiment 5
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) by polyethylene polyamine 253.5g (pentaethylene hexamine, each 0.5mol of six ethylene, seven amine) and catalyst potassium hydroxide
2.5g is added in autoclave, and when being warming up to 100 ± 5 DEG C, pumping it to gauge pressure with vacuum pump is -0.08MPa, uses nitrogen
Scavenging pipeline and reaction kettle 2 times, stir and heat up, when temperature rises to 130 ± 5 DEG C, be slowly added to propylene oxide 1479g
(25.5mol) controls 140 ± 5 DEG C of reaction temperature, and charging rate is to maintain 0.25 ± 0.05MPa of gauge pressure, end of reaction, then delays
It is slow that ethylene oxide 1870g (42.5mol) is added, 140 ± 5 DEG C of reaction temperature are controlled, end of reaction is cooled to room temperature, and is obtained light
Yellow liquid product；
2) above-mentioned product 362g is weighed, dehydrated alcohol 100g and water 300g is added, chloromethanes 52.8g is added dropwise, is warming up to 60
DEG C back flow reaction 3h, cooling obtain transparent clay stabilizer.
Embodiment 6
The structural formula of oil-gas field fracturing clay stabilizer is as follows in the present embodiment:
Its preparation step includes:
1) by polyethylene polyamine 253.5g (pentaethylene hexamine, each 0.5mol of six ethylene, seven amine) and catalyst potassium hydroxide
2.5g is added in autoclave, and when being warming up to 100 ± 5 DEG C, pumping it to gauge pressure with vacuum pump is -0.08MPa, uses nitrogen
Scavenging pipeline and reaction kettle 2 times, stir and heat up, when temperature rises to 130 ± 5 DEG C, be slowly added to ethylene oxide 1496g
(34mol) controls 140 ± 5 DEG C of reaction temperature, and to maintain 0.25 ± 0.05MPa of gauge pressure, end of reaction slowly adds charging rate
Enter propylene oxide 1479g (25.5mol), controls 140 ± 5 DEG C of reaction temperature, end of reaction is slow added into ethylene oxide
1496g (34mol) controls 140 ± 5 DEG C of reaction temperature, and end of reaction is cooled to room temperature, and obtains faint yellow liquid product；
2) above-mentioned product 472g is weighed, isopropanol 300g and water 450g is added, sodium chloroacetate 99g is added dropwise, is warming up to 60 DEG C
Back flow reaction 3h, cooling obtain transparent clay stabilizer.
Test example
1, prevent swollen performance test
Clay stabilizer prepared by Example 1~6, according to People's Republic of China (PRC) oil and gas industry standard SY/T
5971-94 water filling measures anti-dilative with clay stabilizer method of evaluating performance, according to China PetroChemical Corporation standard Q/
SH 0053-2010 clay stabilizer technical requirements measure water-fastness rate, as a result see the table below 1.
Clay stabilizer prevents swollen the performance test results in 1 Examples 1 to 6 of table
As shown in Table 1, clay stabilizer has and excellent prevents swollen performance in Examples 1 to 6.
2, compatibility is tested
Clay stabilizer prepared by Example 1~6, (+1% clay stabilization of 0.3% thickening agent is compounded with commercially available thickening agent
Agent, surplus are water), its compatibility is investigated, as a result see the table below 2.
The compatibility evaluation result of clay stabilizer and commercially available thickening agent in 2 Examples 1 to 6 of table
As shown in Table 2, clay stabilizer and non-ionic hydroxypropyl guar gum, anionic polyacrylamide in Examples 1 to 6
Occur after amine, cationic-type polyacrylamide class thickener compounding without floccule or flocculation phenomenon, compatibility is good.
Claims (10)
1. oil-gas field fracturing clay stabilizer, it is characterised in that: the general structure of the clay stabilizer is as follows:
In formula 2: A is polyoxyethylene groups, and B is polyoxypropylene base, and x, y take any integer in 0~10 respectively, and z takes any in 2~10
Integer；R is the hydroxyalkyl or-CH of hydrogen, the alkyl of 1~5 carbon, 1~5 carbon2-COONa；N takes any integer in 2~5.
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 0~
Any integer in 4, z take 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 that 0 or 3, z is taken to take 4 or 5, the R to be
Hydrogen or methyl.
4. clay stabilizer according to claim 3, it is characterised in that: in formula 2, it is first that x, which takes 0, y that 0 or 3, z is taken to take 5, R,
Base.
5. the preparation method of clay stabilizer as described in any one of Claims 1 to 4, it is characterised in that: with polyethylene polyamine
Ethylene oxide progress is added after ethylene oxide and/or propylene oxide progress open loop addition are added according to actual needs for initiator
Then open loop addition carries out the positive ionization of amine.
6. preparation method according to claim 5, it is characterised in that: the general structure of the polyethylene polyamine is as follows:
In formula 3: n takes any integer in 2~5.
7. preparation method according to claim 6, it is characterised in that: the polyethylene polyamine and ethylene oxide and/or ring
The molar ratio of Ethylene Oxide is 1:(n+4) × (x+y+z).
8. preparation method according to claim 7, it is characterised in that: the cationoid reaction are as follows: obtained by open loop addition
Solvent and cationic reagent are added in product, 0.5~15h is reacted at 25~100 DEG C of temperature.
9. preparation method according to claim 8, it is characterised in that: the cationic reagent is formic acid, acetic acid, phosphorus
Acid, citric acid, the alkyl halide of 1~5 carbon, the halohydrin of 1~5 carbon or 2~5 carbon halogenated carboxylic acid salt.
10. preparation method according to claim 8, it is characterised in that: the solvent is ethyl alcohol, isopropanol or ethylene glycol
Aqueous solution.
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| WO2018104133A1 (en) * | 2016-12-09 | 2018-06-14 | Evonik Degussa Gmbh | 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 | Salt-tolerant clay stabilizer for preparing fracturing fluid from oilfield effluent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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 |
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