CN108485636A - A kind of heat safe nanometer zirconium borate crosslinker and preparation method thereof - Google Patents
A kind of heat safe nanometer zirconium borate crosslinker and preparation method thereof Download PDFInfo
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- CN108485636A CN108485636A CN201810335369.6A CN201810335369A CN108485636A CN 108485636 A CN108485636 A CN 108485636A CN 201810335369 A CN201810335369 A CN 201810335369A CN 108485636 A CN108485636 A CN 108485636A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
Abstract
The invention discloses a kind of heat safe nanometer zirconium borate crosslinkers and preparation method thereof.The preparation method of the crosslinking agent is：(1) sodium dodecyl sulfate solution and eight water zirconyl chloride solutions is respectively configured；(2) eight water zirconyl chloride solutions are added dropwise in sodium dodecyl sulfate solution, add hexamethylene, then places it in reaction kettle, sodium hydroxide solution is added, reaction for 24 hours, obtains nano zirconium dioxide emulsion；(3) glycerine, borax, beta diketone and triethanolamine are sequentially added into nano zirconium dioxide emulsion, are reacted under conditions of being 10 in pH value, a nanometer zirconium borate crosslinker is prepared.The nanometer zirconium borate crosslinker that the method for the present invention is prepared not only has excellent heatproof endurance of cutting, but also at low cost, and fragile glue returns row.
Description
Technical field
The invention belongs to oil field crosslinking agent preparing technical fields, and in particular to a kind of heat safe nanometer zirconium borate crosslinker
And preparation method thereof.
Background technology
Petroleum resources pass through the exploitation of decades, and most Thief zone oil gas field has come into the exploitation later stage.In order to
Improve stratum permeability and improve Oil ＆ Gas Productivity, stratum modification measures are essential.Pressure break is caused as deep low-permeability
The maximally efficient stratum modification measures of close property reservoir receive more and more concerns and research both at home and abroad.Crosslinking agent is to influence
One of the main determining factor of pressing crack construction success or not.
And currently, common crosslinking agent is organic borate cross-linker in oil field, but there are resistance to for existing organic borate cross-linker
The problem of hot difference, the temperature tolerance for the organic borate cross-linker that many oil gas fields use are only capable of reaching 120 DEG C or so, the temperature used
No more than 150 DEG C, the pressing crack construction of deep-well is not adapted to.
In addition, the preparation principle of existing organic boron zirconium cross linking agent is matched using metal ion and borax, polyalcohol etc.
Body complex reaction and be made.This method increases exoil field cost there are metal ion dosage is larger, is unfavorable for the crosslinking of organic boron zirconium
Agent is popularized.Furthermore the preparation method of organic boron zirconium cross linking agent is more demanding, and technological requirement is stringent, it is unfavorable for the friendship of organic boron zirconium
Join the industrialized production of agent.
Invention content
For above-mentioned deficiency in the prior art, a kind of heat safe nanometer zirconium borate crosslinker of present invention offer and its preparation
Method can effectively solve the problems, such as existing crosslinking agent non-refractory, of high cost.
To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is：
A kind of preparation method of heat safe nanometer zirconium borate crosslinker, includes the following steps：
(1) in the sodium dodecyl sulfate solution that 40~45 DEG C of configuration concentrations are 0.1~0.5g/mL, then at normal temperatures
Configuration concentration is the eight water zirconyl chloride solutions of 0.1~0.25g/mL；
(2) eight water zirconyl chloride solutions are added dropwise in sodium dodecyl sulfate solution, are stirred, add hexamethylene
Alkane, 2~3h of magnetic agitation；Wherein, the volume ratio of sodium dodecyl sulfate solution, eight water zirconyl chloride solutions and hexamethylene is 1
~2:1:2~5；
(3) step (2) products therefrom is placed in reaction kettle, sodium hydroxide solution is then added, it is anti-in 100~120 DEG C
24~28h is answered, washs 2~3 times, obtains nano zirconium dioxide emulsion；
(4) then ultrasonic disperse nano zirconium dioxide emulsion is added and accounts for the third the three of its volume 35%~50% thereto
Alcohol is stirred, and adds borax, and in 40~45 DEG C of stirring and dissolvings, regulation system pH value is 10~11, and anti-in 60~65 DEG C
5~8h is answered, beta-diketon and triethanolamine are finally added, the reaction was continued 5~8h obtains a nanometer zirconium borate crosslinker；Wherein, borax with
The weight ratio of eight water oxygen zirconium chlorides is 1.5~2.5:1；The volume ratio of beta-diketon, triethanolamine and glycerine is 0.1~0.5:
0.8~1.5:1.
Wherein, nanometer zirconium borate crosslinker preparating mechanism is as follows：
The first step：Nano zirconium dioxide is reacted with borax generates boric acid ester compound；
Second step：Borate is reacted with beta-diketon and triacetamide is made nanometer zirconium borate crosslinker；
Further, in step (1) sodium dodecyl sulfate solution a concentration of 0.1~0.15g/mL.
Further, in step (1) eight water zirconyl chloride solutions a concentration of 0.1~0.2g/mL.
Further, in step (2) sodium dodecyl sulfate solution, eight water zirconyl chloride solutions and hexamethylene volume ratio
It is 2:1:5.
Further, the volume ratio of sodium hydroxide solution and eight water zirconyl chloride solutions is 2:1, and sodium hydroxide solution
A concentration of 4mol/L.
Further, washing process is in step (3)：With alternately washing 3 times of ethyl alcohol and deionized water.
Further, the volume ratio of glycerine and nano zirconium dioxide emulsion is 1 in step (4):2.
Further, the weight ratio of borax and eight water oxygen zirconium chlorides is 2.2~2.5 in step (4):1.
Further, the volume ratio of beta-diketon, triethanolamine and glycerine is 0.16 in step (4):1.2:1.
The nanometer zirconium borate crosslinker being prepared into using the above method.
The method of the present invention has the beneficial effect that：
1, nano zirconium dioxide is prepared by the method for the invention, and easy to operate, simple and practicable, cost of material is low, to behaviour
The harm for making personnel is low, meanwhile, the nano zirconium dioxide surface being prepared has a large amount of hydroxyl, has good hydrophilic
Property, subsequently to have established good chemical basis with reacting for substances such as boraxs.
2, nanometer zirconium borate crosslinker preparation method is simple, easy to operation, in preparation process, without using nitrogen or ammonia
As protection gas, easy to produce, cost is relatively low, also, also introducing has nano zirconium dioxide in crosslinking agent, takes full advantage of and receives
The advantages such as the multidigit point of rice zirconium oxide so that crosslinking agent has good heatproof endurance of cutting.
3, nanometer zirconium borate crosslinker appearance is weak yellow liquid, and stability is good, non-ignitable, not quick-fried, stores transportation safety.
4, the nanometer zirconium borate crosslinker that the method for the present invention is prepared is in crosslinking 0.3wt%HPG, when crosslinking ratio is 1.2%,
At 120 DEG C, 170s-1Under conditions of, viscosity is maintained at 180mpa.s or more；In crosslinking 6wt%HPG, when crosslinking ratio is 0.5%,
1% temperature stability agent is supplemented, at 180 DEG C, 170s-1Under conditions of, viscosity is maintained at 60mpa.s or more, embodies good resistance to
Warm endurance of cutting.
Description of the drawings
Fig. 1 is 0.3wt%HPG, crosslinked gel heatproof resistant to shearing curve when crosslinking ratio is 1.2%；
Fig. 2 is 0.6wt%HPG, crosslinked gel heatproof resistant to shearing curve when crosslinking ratio is 0.5%.
Specific implementation mode
The specific implementation mode of the present invention is described below, in order to facilitate understanding by those skilled in the art this hair
It is bright, it should be apparent that the present invention is not limited to the ranges of specific implementation mode, for those skilled in the art,
As long as various change is in the spirit and scope of the present invention that the attached claims limit and determine, these variations are aobvious and easy
See, all are using the innovation and creation of present inventive concept in the row of protection.
Embodiment 1
A kind of preparation method of heat safe nanometer zirconium borate crosslinker, includes the following steps：
(1) 8.65g lauryl sodium sulfate is taken to be dissolved in 60mL deionized waters, stirring and dissolving under the conditions of 45 DEG C；
(2) it weighs eight water oxygen zirconium chlorides of 4.83g to be dissolved in 30mL deionized waters, stirring at normal temperature dissolving；Under agitation,
Zirconyl chloride solution is slowly dropped in sodium dodecyl sulfate solution, 150mL hexamethylenes, magnetic agitation 2- is then added
3h obtains mixed liquor；
(3) gained mixed liquor is moved in the hydrothermal reaction kettle that 500mL contains polytetrafluoroethyllining lining, addition 60mL,
The sodium hydroxide solution of 4mol/l reacts under the conditions of 100 DEG C for 24 hours, with ethyl alcohol and deionized water alternately washing 3 times, by theoretical production
Rate is made into the nano zirconium dioxide emulsion of 0.5wt%, and ultrasonic 30min makes it be uniformly dispersed；
(4) it takes the nano zirconium dioxide emulsion of 50ml 0.5wt% in three-necked flask, 25mL the third three is added thereto
Alcohol, stirring make it be uniformly mixed, and 12g boraxs are then added, and 40 DEG C of stirring and dissolvings continuously add appropriate sodium hydroxide, by system
PH value is transferred to 10, then is warming up at 60 DEG C and reacts 5h, adds 4mL beta-diketons and 30mL triethanolamines, continues in 60 DEG C of conditions
Lower reaction 5h is to get to the nanometer zirconium borate crosslinker for faint yellow viscous liquid.
Embodiment 2
A kind of preparation method of heat safe nanometer zirconium borate crosslinker, includes the following steps：
(1) 12g lauryl sodium sulfate is taken to be dissolved in 120mL deionized waters, stirring and dissolving under the conditions of 45 DEG C；
(2) it weighs eight water oxygen zirconium chlorides of 8.4g to be dissolved in 60mL deionized waters, stirring at normal temperature dissolving；Under agitation,
Zirconyl chloride solution is slowly dropped in sodium dodecyl sulfate solution, 300mL hexamethylenes, magnetic agitation 2- is then added
3h obtains mixed liquor；
(3) gained mixed liquor is moved in the hydrothermal reaction kettle that 500mL contains polytetrafluoroethyllining lining, addition 60mL,
The sodium hydroxide solution of 4mol/l reacts under the conditions of 100 DEG C for 24 hours, with ethyl alcohol and deionized water alternately washing 3 times, by theoretical production
Rate is made into the nano zirconium dioxide emulsion of 0.5wt%, and ultrasonic 30min makes it be uniformly dispersed；
(4) it takes the nano zirconium dioxide emulsion of 60ml 0.5wt% in three-necked flask, 30mL the third three is added thereto
Alcohol, stirring make it be uniformly mixed, and 18.48g boraxs are then added, and 40 DEG C of stirring and dissolvings continuously add appropriate sodium hydroxide, by body
It is that pH value is transferred to 10, then is warming up at 60 DEG C and reacts 5h, adds 4.8mL beta-diketons and 36mL triethanolamines, continues at 60 DEG C
Under the conditions of reaction 5h to get to the nanometer zirconium borate crosslinker for faint yellow viscous liquid.
Embodiment 3
A kind of preparation method of heat safe nanometer zirconium borate crosslinker, includes the following steps：
(1) 16.2g lauryl sodium sulfate is taken to be dissolved in 90mL deionized waters, stirring and dissolving under the conditions of 45 DEG C；
(2) it weighs eight water oxygen zirconium chlorides of 6.75g to be dissolved in 45mL deionized waters, stirring at normal temperature dissolving；Under agitation,
Zirconyl chloride solution is slowly dropped in sodium dodecyl sulfate solution, 225mL hexamethylenes, magnetic agitation 2- is then added
3h obtains mixed liquor；
(3) gained mixed liquor is moved in the hydrothermal reaction kettle that 500mL contains polytetrafluoroethyllining lining, addition 60mL,
The sodium hydroxide solution of 4mol/l reacts under the conditions of 100 DEG C for 24 hours, with ethyl alcohol and deionized water alternately washing 3 times, by theoretical production
Rate is made into the nano zirconium dioxide emulsion of 0.5wt%, and ultrasonic 30min makes it be uniformly dispersed；
(4) it takes the nano zirconium dioxide emulsion of 50ml 0.5wt% in three-necked flask, 25mL the third three is added thereto
Alcohol, stirring make it be uniformly mixed, and 12g boraxs are then added, and 40 DEG C of stirring and dissolvings continuously add appropriate sodium hydroxide, by system
PH value is transferred to 10, then is warming up at 60 DEG C and reacts 5h, adds 4mL beta-diketons and 30mL triethanolamines, continues in 60 DEG C of conditions
Lower reaction 5h is to get to the nanometer zirconium borate crosslinker for faint yellow viscous liquid.
Detection
Under identical conditions, nanometer zirconium borate crosslinker and existing organic borate cross-linker are prepared to embodiment 1 respectively
It is detected, by testing result it is found that the temperature tolerance of existing organic borate cross-linker when in use is only capable of reaching 120 DEG C of left sides
The right side, and heatproof the shearing curve such as Fig. 1 and figure for the nanometer zirconium borate crosslinker being prepared using 1 the method for the embodiment of the present invention
Shown in 2；
According to the heatproof shearing curve of Fig. 1 and Fig. 2 it is found that the nanometer zirconium borate crosslinker that the method for the present invention is prepared is being handed over
Join 0.3wt%HPG, when crosslinking ratio is 1.2%, at 120 DEG C, 170s-1Under conditions of, viscosity is maintained at 180mpa.s or more；
It is crosslinked 6wt%HPG, when crosslinking ratio is 0.5%, supplements 1% temperature stability agent, at 180 DEG C, 170s-1Under conditions of, viscosity is kept
In 60mpa.s or more, good heatproof endurance of cutting is embodied.
Claims (10)
1. a kind of preparation method of heat safe nanometer zirconium borate crosslinker, which is characterized in that include the following steps：
(1) it in the sodium dodecyl sulfate solution that 40~45 DEG C of configuration concentrations are 0.1~0.5g/mL, then configures at normal temperatures
The eight water zirconyl chloride solutions of a concentration of 0.1~0.25g/mL；
(2) eight water zirconyl chloride solutions are added dropwise in sodium dodecyl sulfate solution, are stirred, add hexamethylene, magnetic
Power stirs 2~3h；Wherein, the volume ratio of sodium dodecyl sulfate solution, eight water zirconyl chloride solutions and hexamethylene is 1~2:1:
2~5；
(3) step (2) products therefrom is placed in reaction kettle, sodium hydroxide solution is then added, react 24 in 100~120 DEG C
~28h washs 2~3 times, obtains nano zirconium dioxide emulsion；
(4) then ultrasonic disperse nano zirconium dioxide emulsion is added the glycerine for accounting for its volume 35%~50%, stirs thereto
Mixing is mixed, borax is added, in 40~45 DEG C of stirring and dissolvings, regulation system pH value is 10~11, and react in 60~65 DEG C 5~
8h finally adds beta-diketon and triethanolamine, the reaction was continued 5~8h, obtains a nanometer zirconium borate crosslinker；Wherein, borax and eight water
The weight ratio of zirconium oxychloride is 1.5~2.5:1；The volume ratio of beta-diketon, triethanolamine and glycerine is 0.1~0.5:0.8~
1.5:1。
2. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (1)
Described in sodium dodecyl sulfate solution a concentration of 0.1~0.15g/mL.
3. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (1)
Described in eight water zirconyl chloride solutions a concentration of 0.1~0.2g/mL.
4. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (2)
Described in sodium dodecyl sulfate solution, eight water zirconyl chloride solutions and hexamethylene volume ratio be 2:1:5.
5. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (3)
Described in the volume ratios of sodium hydroxide solution and eight water zirconyl chloride solutions be 2:1, and a concentration of 4mol/ of sodium hydroxide solution
L。
6. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (3)
Described in washing process be：With alternately washing 3 times of ethyl alcohol and deionized water.
7. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (4)
Described in the volume ratio of glycerine and nano zirconium dioxide emulsion be 1:2.
8. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (4)
Described in the weight ratios of borax and eight water oxygen zirconium chlorides be 2.2~2.5:1.
9. the preparation method of heat safe nanometer zirconium borate crosslinker according to claim 1, which is characterized in that step (4)
Described in beta-diketon, triethanolamine and glycerine volume ratio be 0.16:1.2:1.
10. the nanometer zirconium borate crosslinker being prepared using any one of claim 1~9 the method.
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| CN114410287A (en) * | 2021-12-31 | 2022-04-29 | 宁波锋成先进能源材料研究院有限公司 | Composite nano cross-linking agent and preparation method and application thereof |
| CN114410287B (en) * | 2021-12-31 | 2023-08-08 | 宁波锋成先进能源材料研究院有限公司 | Composite nano cross-linking agent and preparation method and application thereof |
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