CN108048069A - A kind of preparation method of high temperature resistant fracturing fluid compositions - Google Patents
A kind of preparation method of high temperature resistant fracturing fluid compositions Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high temperature resistant fracturing fluid compositions, detailed process is：Maleic anhydride modified guanidine glue is prepared first, then acrylic amine monomer, acrylic acid, methacrylic acid are mixed to join N, initiator is continuously added after being stirred in N-dimethylformamide, reaction, it is cooled to room temperature after reaction, product obtained and maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material；Organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine are sequentially added into mixed material obtained above, nano-titanium oxide, ammonium sulfate are added in after being uniformly mixed, fracturing fluid compositions are made after being stirred.Fracturing fluid compositions stability produced by the present invention is good, and high temperature resistance is excellent, and manufacturing cost is low.
Description
Technical field：
The present invention relates to oilfield exploitation technologies, are specifically related to a kind of preparation method of high temperature resistant fracturing fluid compositions.
Background technology：
In general, the abundance of low-permeability oil deposit is low, reservoir permeability the characteristics of also single well productivity is relatively low.Simultaneously
With high permeable cement in contrast, the density of crude oil is relatively small, viscosity is relatively low, and low-permeability oil deposit fluid flows
When, non-darcy feature is apparent.The cement content of low-permeability oil deposit is relatively large, and the law of development of sand body is relatively small, and
Oil reservoir and sand shale interaction, the thickness stability for causing layer of sand are inadequate.After oil reservoir water breakthrough, productivity index and fluid productivity index can
It significantly decreases, this will cause very big adverse effect to the stable yields in oil field to a certain extent.To improve hyposmosis
The oil productivity of oil reservoir, fracturing fluid become one of key.
Chinese patent 201410396894.0 discloses a kind of complex thickener fracturing fluid, component and weight percent
For：Hydroxypropyl guar：0.1%-0.3%, modified starch：2%-4%；Clay stabilizer：0.5%-2%, temperature stability agent：
0.1%-0.5%, cleanup additive：0.1%-1%, fungicide：0.1%-0.3%, pH adjusting agent：0.1%-0.3%, surplus are
Water；The preparation of the modified starch：Cured matter starch is carried out by acetylated modification using acetic anhydride first, then using three metaphosphoric acids
Sodium or phosphorus oxychloride carry out phosphorylation modification to it, and spray drying is finally carried out to modified product and carries out pre-gelatinized processing.Although
Fracturing fluid is at low cost made from this method, but its stability is poor, and in use, residue is more.Chinese patent
200910216753.5 disclose fracturing fluid additive, mainly solve fracturing fluid in the prior art and are difficult to meet environmental requirement
Problem.The cross-linked oil-in-water emulsified fracturing fluid additive, which is characterized in that including emulsifier, thickening agent, crosslinking agent, filtrate reducing
Agent, gel breaker, cleanup additive, clay stabilizer, mass ratio 7: 4: 4: 50: 3: 2: 30.The present invention can be largely
The using effect of fracturing fluid is improved, fracturing fluid is made thoroughly to break glue, and increases cementability.But it cannot still change fracturing fluid
High temperature resistance and can't resolve the problem of residue after pressing crack construction is more.
The content of the invention：
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of preparation sides of high temperature resistant fracturing fluid compositions
Method, this method is easy to operate, and manufacturing cost is low, and fracturing fluid stability obtained is good, and high temperature resistance is excellent.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, adding in acidic catalyst after reaction, the reaction was continued, and maleic anhydride modified guanidine glue is made；
(2) acrylic amine monomer, acrylic acid, methacrylic acid are weighed and is mixed to join N, stirred in N-dimethylformamide
Initiator is continuously added after mixing, 5-8h is reacted at 60-80 DEG C, is cooled to room temperature after reaction, by product obtained and
Maleic anhydride modified guanidine glue mixing obtained above, obtains mixed material；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred.
As the preferred of above-mentioned technical proposal, in step (1), the maleic anhydride, the mass ratio of guanidine glue are (0.06-
0.08)：1.
As the preferred of above-mentioned technical proposal, in step (1), the acidic catalyst is the concentrated sulfuric acid, boron trifluoride, poly
One or more mixing in phosphoric acid.
As the preferred of above-mentioned technical proposal, in step (1), the additive amount of the acidic catalyst is guanidine colloid amount
0.5%-1%.
As the preferred of above-mentioned technical proposal, in step (2), each component is respectively in parts by weight：Acrylic amine
20-40 parts of monomer, 15-20 parts of acrylic acid, 10-20 parts of methacrylic acid, N, 10-15 parts of N-dimethylformamide, initiator 1-
1.5 parts, 1-3 parts of maleic anhydride modified guanidine glue.
As the preferred of above-mentioned technical proposal, in step (2), the initiator is ammonium persulfate, one in potassium peroxydisulfate
Kind.
As the preferred of above-mentioned technical proposal, in step (1), the time of the reaction is 1-4h.
As the preferred of above-mentioned technical proposal, in step (3), the heat stabilizer is sodium thiosulfate, diethanol amine, neighbour
One kind in phenylenediamine.
As the preferred of above-mentioned technical proposal, the maleic anhydride modified guanidine glue, organic boron zirconium cross linking agent, heat stabilizer,
Azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：(0.5-0.8)：(0.7-1)：0.5：(0.1-0.3)：
(0.01-0.05)。
The invention has the advantages that：
Fracturing fluid high temperature resistance of the prior art is poor, and residue is more in the construction process asks from solving by the present invention
Topic, using maleic anhydride modified guanidine glue, prepare it is relatively simple, using ethyl alcohol as reaction medium in preparation process, with maleic anhydride
It is reaction raw materials with guanidine glue, is reacted under conditions of acidic catalyst catalysis, the reaction condition is mild, at low cost, is easy to
Operation, compared with the modification technology of the prior art to guanidine glue, present invention process is relatively simple, low for equipment requirements；
Fracturing fluid produced by the present invention has good dissolubility, can quickly dissolve, and when fracturing fluid viscosity can be long
Between keep stablize, improve site operation efficiency.
Specific embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in the concentrated sulfuric acid the reaction was continued 1h after reaction, and maleic anhydride modified guanidine glue is made；Its
In, maleic anhydride, the mass ratio of guanidine glue are 0.06：1；The additive amount of the concentrated sulfuric acid is the 0.5% of guanidine colloid amount；
(2) 20 parts of acrylic amine monomers, 15 parts of acrylic acid, 10 parts of methacrylic acids are weighed and is mixed to join 10 parts of N, N bis-
1 part of initiator is continuously added after being stirred in methylformamide, 5h is reacted at 60 DEG C, is cooled to room temperature after reaction,
Product obtained and 1 part of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.5:0.7：0.5：0.1：0.01.
Embodiment 2
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in polyphosphoric acids the reaction was continued 4h after reaction, and maleic anhydride modified guanidine glue is made；
Wherein, maleic anhydride, the mass ratio of guanidine glue are 0.08：1；The additive amount of polyphosphoric acids is the 1% of guanidine colloid amount；
(2) 40 parts of acrylic amine monomers, 20 parts of acrylic acid, 20 parts of methacrylic acids are weighed and is mixed to join 15 parts of N, N bis-
1.5 parts of initiators are continuously added after being stirred in methylformamide, 8h is reacted at 80 DEG C, is cooled to room after reaction
Product obtained and 3 parts of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material by temperature；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.8：1：0.5：0.3：0.05.
Embodiment 3
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in boron trifluoride the reaction was continued 2h after reaction, and maleic anhydride modified guanidine glue is made；
Wherein, maleic anhydride, the mass ratio of guanidine glue are 0.065：1；The additive amount of boron trifluoride is the 0.6% of guanidine colloid amount；
(2) 24 parts of acrylic amine monomers, 16 parts of acrylic acid, 12 parts of methacrylic acids are weighed and is mixed to join 11 parts of N, N bis-
1.1 parts of initiators are continuously added after being stirred in methylformamide, 6h is reacted at 65 DEG C, is cooled to room after reaction
Product obtained and 1.5 parts of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material by temperature；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.55：0.75：0.5：0.15：0.02.
Embodiment 4
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in the concentrated sulfuric acid the reaction was continued 2h after reaction, and maleic anhydride modified guanidine glue is made；Its
In, maleic anhydride, the mass ratio of guanidine glue are 0.065：1；The additive amount of the concentrated sulfuric acid is the 0.8% of guanidine colloid amount；
(2) 28 parts of acrylic amine monomers, 17 parts of acrylic acid, 14 parts of methacrylic acids are weighed and is mixed to join 13 parts of N, N bis-
1.2 parts of initiators are continuously added after being stirred in methylformamide, 6h is reacted at 70 DEG C, is cooled to room after reaction
Product obtained and 2 parts of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material by temperature；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.6：0.8：0.5：0.2：0.03.
Embodiment 5
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in the concentrated sulfuric acid the reaction was continued 3h after reaction, and maleic anhydride modified guanidine glue is made；Its
In, maleic anhydride, the mass ratio of guanidine glue are 0.07：1；The additive amount of the concentrated sulfuric acid is the 0.7% of guanidine colloid amount；
(2) 30 parts of acrylic amine monomers, 18 parts of acrylic acid, 16 parts of methacrylic acids are weighed and is mixed to join 13 parts of N, N bis-
1.3 parts of initiators are continuously added after being stirred in methylformamide, 6h is reacted at 70 DEG C, is cooled to room after reaction
Product obtained and 2 parts of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material by temperature；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.65：0.7：0.5：0.2：0.03.
Embodiment 6
A kind of preparation method of high temperature resistant fracturing fluid compositions, comprises the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, add in polyphosphoric acids the reaction was continued 3.5h after reaction, and maleic anhydride modified guanidine is made
Glue；Wherein, maleic anhydride, the mass ratio of guanidine glue are 0.075：1；The additive amount of polyphosphoric acids is the 0.8% of guanidine colloid amount；
(2) 35 parts of acrylic amine monomers, 18 parts of acrylic acid, 18 parts of methacrylic acids are weighed and is mixed to join 14 parts of N, N bis-
1.4 parts of initiators are continuously added after being stirred in methylformamide, 7h is reacted at 75 DEG C, is cooled to room after reaction
Product obtained and 2 parts of maleic anhydride modified guanidine glue obtained above are mixed, obtain mixed material by temperature；
(3) organic boron zirconium cross linking agent, heat stabilizer, sulfopropyl beet are sequentially added into mixed material obtained above
Alkali adds in nano-titanium oxide, ammonium sulfate after being uniformly mixed, fracturing fluid compositions are made after being stirred；Wherein, maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
0.75：0.8：0.5：0.3：0.04.
Comparative example
Using guanidine glue in fracturing fluid, maleic anhydride is not used to be modified, other conditions and embodiment 6 are identical.
After testing, the fracturing fluid residue content measuring in 1-6 of the embodiment of the present invention is 3.5-5.5%, and in comparative example
Residue content test is 18.1%, and for comparative example, the stability of fracturing fluid produced by the present invention is more preferable, residue content
It substantially reduces.
Moreover, fracturing fluid produced by the present invention is in 170 DEG C, 170s-1Condition down cut 60min, viscosity are maintained at 75mPa
More than s.Live needs can be fully met.
Claims (9)
1. a kind of preparation method of high temperature resistant fracturing fluid compositions, which is characterized in that comprise the following steps：
(1) maleic anhydride and absolute ethyl alcohol are mixed and mixed liquor is made, then add in ultrasound under guanidine glue 500W power
Then 10min reacts at 60 DEG C, adding in acidic catalyst after reaction, the reaction was continued, and maleic anhydride modified guanidine glue is made；
(2) acrylic amine monomer, acrylic acid, methacrylic acid are weighed and is mixed to join N, be stirred in N-dimethylformamide
After continuously add initiator, 5-8h is reacted at 60-80 DEG C, is cooled to room temperature after reaction, by product obtained and above-mentioned
Maleic anhydride modified guanidine glue mixing obtained, obtains mixed material；
(3) organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine are sequentially added into mixed material obtained above, is stirred
It mixes and adds in nano-titanium oxide, ammonium sulfate after mixing, fracturing fluid compositions are made after being stirred.
2. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (1),
The maleic anhydride, the mass ratio of guanidine glue are (0.06-0.08)：1.
3. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (1),
The acidic catalyst is the concentrated sulfuric acid, one or more mixing in boron trifluoride, polyphosphoric acids.
4. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (1),
The additive amount of the acidic catalyst is the 0.5%-1% of guanidine colloid amount.
5. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (2),
The each component is respectively in parts by weight：20-40 parts of acrylic amine monomer, 15-20 parts of acrylic acid, methacrylic acid 10-20
Part, N, 10-15 parts of N-dimethylformamide, 1-1.5 parts of initiator, 1-3 parts of maleic anhydride modified guanidine glue.
6. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (2),
The initiator is ammonium persulfate, one kind in potassium peroxydisulfate.
7. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (1),
The time of the reaction is 1-4h.
8. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：In step (3),
The heat stabilizer is sodium thiosulfate, one kind in diethanol amine, o-phenylenediamine.
9. a kind of preparation method of high temperature resistant fracturing fluid compositions as described in claim 1, it is characterised in that：The maleic acid
Anhydride modification guanidine glue, organic boron zirconium cross linking agent, heat stabilizer, azochlorosulfonate propyl lycine, nano-titanium oxide, the mass ratio of ammonium sulfate are 1：
(0.5-0.8)：(0.7-1)：0.5：(0.1-0.3)：(0.01-0.05).
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| CN109957041A (en) * | 2019-04-23 | 2019-07-02 | 绿新（福建）食品有限公司 | A kind of comprehensive method for improving carragheen quality |
| CN110819323A (en) * | 2019-11-26 | 2020-02-21 | 陕西科技大学 | Fluorine-containing temporary plugging type cleanup additive particle and preparation method and application thereof |
| CN116285936A (en) * | 2023-03-15 | 2023-06-23 | 成都劳恩普斯科技有限公司 | High-temperature-resistant salt-resistant instant fracturing fluid thickener and preparation method thereof |
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2017
- 2017-12-29 CN CN201711489163.0A patent/CN108048069A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957041A (en) * | 2019-04-23 | 2019-07-02 | 绿新（福建）食品有限公司 | A kind of comprehensive method for improving carragheen quality |
| CN110819323A (en) * | 2019-11-26 | 2020-02-21 | 陕西科技大学 | Fluorine-containing temporary plugging type cleanup additive particle and preparation method and application thereof |
| CN110819323B (en) * | 2019-11-26 | 2022-04-12 | 陕西科技大学 | Fluorine-containing temporary plugging type cleanup additive particle and preparation method and application thereof |
| CN116285936A (en) * | 2023-03-15 | 2023-06-23 | 成都劳恩普斯科技有限公司 | High-temperature-resistant salt-resistant instant fracturing fluid thickener and preparation method thereof |
| CN116285936B (en) * | 2023-03-15 | 2024-05-24 | 成都劳恩普斯科技有限公司 | High-temperature-resistant salt-resistant instant fracturing fluid thickener and preparation method thereof |
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