CN106318368B - A kind of preparation method of lye control release type nano oxygen agent microcapsules - Google Patents

A kind of preparation method of lye control release type nano oxygen agent microcapsules Download PDF

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Publication number
CN106318368B
CN106318368B CN201610680035.3A CN201610680035A CN106318368B CN 106318368 B CN106318368 B CN 106318368B CN 201610680035 A CN201610680035 A CN 201610680035A CN 106318368 B CN106318368 B CN 106318368B
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oxidant
microcapsules
mass ratio
certain mass
alcohol
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CN106318368A (en
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左明明
裴思静
左晓兵
陈奠宇
曹振兴
罗铭
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Changshu Institute of Technology
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Changshu Institute of Technology
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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
    • C09K8/70—Compositions for forming crevices or fractures characterised by their form or by the form of their components, e.g. foams
    • C09K8/706—Encapsulated breakers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/26—Gel breakers other than bacteria or enzymes

Abstract

The invention discloses a kind of preparation methods of lye control release type nano oxygen agent microcapsules, include the following steps：(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, is stirred to react a period of time；(2) oxidant, epoxy resin, polyamide and the silica of certain mass ratio is added, the reaction was continued a period of time；(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, continues to be stirred to react a period of time, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.The preparation method of lye control release type nano oxygen agent microcapsules provided by the invention, there is oxidant microcapsules obtained timing to concentrate release function, while the concentration that its starting release time controllably overregulates lye carrys out accuracy controlling.

Description

A kind of preparation method of lye control release type nano oxygen agent microcapsules
Technical field
The present invention relates to the volume increase of the oil-water wells such as oil field development technical field, especially microcapsule degelling agent, profile-controlling and plugging agent A kind of increase water injection technology field, and in particular to preparation method of lye control release type nano oxygen agent microcapsules.
Background technique
Microcapsules technology refer to natural or synthetic macromolecule coating material by the solid material with certain dispersibility, Fluent material or gas wrapping get up, and form a kind of fine particle with obvious " core-shell structure copolymer " structure, and the fine particle is referred to as micro- Capsule.Commonly referred to as coating material is cyst wall or wall material, and the substance for being coated material package is known as capsule-core or core material.Prepared is micro- The properties such as capsule size, shape and controlled release properties and preparation process, the selection of raw material, the parameters such as size of core material are closely related, And its change of properties range of the microcapsules prepared under different conditions is larger.It can be incited somebody to action according to the property of microcapsules coating material Microcapsules are divided into organic or inorganic coating microcapsules；Microcapsules can be divided into full infiltration according to the permeability of microcapsule wall material Thoroughly, the microcapsules of semi-permeable, impermeable three types can additionally see releasing for core material in microcapsules according to the permeability of coating The mode of putting is slow or burst release.
Oxidant (such as ammonium persulfate, potassium peroxydisulfate, chromium trichloride, sodium dichromate, potassium bichromate, potassium permanganate) microcapsules It is widely used in oilfield at present：Gel breaker as oil field fracturing fluid can solve to keep pressure in oil field compression fracture work progress Glue is broken after splitting fluid viscosity and construction returns the difficult problem of row；Oxidant microcapsules are applied to by polyacrylamide (HPAM)- When can get plastic in the profile-controlling and plugging agent system of high volence metal ion [such as Cr (III), Al (III), Zr (IV)] system composition Between the high profile-controlling and plugging agent of intensity after long and plastic.
The composition of microcapsule membrane material is the key factor for determining microcapsules storage stability, release time and mode, often There is gelatin, Arabic gum, sodium alginate, ethyl cellulose, chitosan, solid paraffin, poly- as oxidant microcapsules membrane material The natural or synthetic high molecular material such as vinyl chloride.It is different by the generation type of microcapsules membrane material, it can be used for oxidant microcapsules Preparation method have spray drying process, solvent evaporated method, oil-phase separating method, fusing dispersion condensation method etc..Select above-mentioned membrane material and Different shapes and sizes and the microcapsules with slow-release function can be successfully made in preparation method, however are but difficult to prepare release time Release type microcapsules are concentrated in controllable timing.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of lye control release type nano oxygen agent is micro- The preparation method of capsule.
For the purpose of the present invention, technical solution provided by the invention is：
A kind of preparation method of lye control release type nano oxygen agent microcapsules, includes the following steps：
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, is stirred to react a period of time；
(2) be added certain mass ratio oxidant, epoxy resin, polyamide and silica, the reaction was continued one section Time；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, continues to be stirred to react a period of time, deionization Water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
In some embodiments wherein, the oxidant, oleic acid, lauryl alcohol, epoxy resin, polyamide, two Silica, ethylenediamine, ethyl alcohol, ethyl acetate account for respectively the total weight that feeds intake 5%~8%, 0.5%~0.9%, 0.4%~ 5%~8%, 3%~5%, 0.1%~0.3%, 0.04%~0.07%, 0.8%~1.2%, 75.93% 0.6% ,~ 85.16%.
In some embodiments wherein, the oxidant is ammonium persulfate, potassium peroxydisulfate, chromium trichloride, dichromic acid One of sodium, potassium bichromate, potassium permanganate.
In some embodiments wherein, the reaction time is 5~6min in the step (1).
In some embodiments wherein, the reaction time is 40~50min in the step (2).
In some embodiments wherein, the reaction time is 12~14h in the step (3).
Scheme in compared with the existing technology, it is an advantage of the invention that：
Using technical solution of the present invention, there is oxidant microcapsules obtained timing to concentrate release function, and this is micro- The release time of capsule can be by adjusting the concentration of lye come accuracy controlling.
Detailed description of the invention
Fig. 1 a is the scanning electron microscope (SEM) photograph of oxidant microcapsules in embodiment 1.
Fig. 1 b is the scanning electron microscope enlarged drawing of oxidant surface of microcapsule in embodiment 1.
Fig. 1 c is the transmission electron microscope picture of oxidant microcapsules in embodiment 1.
Fig. 2 is the release time of oxidant microcapsules in embodiment 1 with concentration of lye variation diagram.
Specific embodiment
Above scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating The present invention and be not limited to limit the scope of the invention.Implementation condition used in the examples can be done according to the condition of specific producer Further adjustment, the implementation condition being not specified is usually the condition in routine experiment.
Embodiment 1：
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, oleic acid, lauryl alcohol, acetic acid second Ester accounts for 0.5%, 0.4%, the 85.16% of the total amount that feeds intake respectively, is stirred to react 5~6min；
(2) ammonium persulfate, epoxy resin, polyamide and the silica of certain mass ratio, ammonium persulfate, ring is added Oxygen resin, polyamide, silica account for 5%, 5%, 3%, the 0.1% of the total amount that feeds intake respectively, and the reaction was continued 40~ 50min；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, ethylenediamine, ethyl alcohol account for the total amount that feeds intake respectively 0.04%, 0.8%, continue to be stirred to react 12~14h, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
Fig. 1 a is the scanning electron microscope (SEM) photograph of oxidant microcapsules in embodiment 1；Fig. 1 b is oxidant microcapsules table in embodiment 1 The scanning electron microscope enlarged drawing in face；Fig. 1 c is the transmission electron microscope picture of oxidant microcapsules in embodiment 1.From Fig. 1 a：It is made Standby oxidant Microcapsules Size is at 13 μm or so, and surface is in the form of coarse.From Fig. 1 b：Oxidant surface of microcapsule It is made of a large amount of nano particle, it is contemplated that nano silica is successfully entrained in polymer membrane material.From Fig. 1 c： Prepared oxidant microcapsules are in apparent " core-shell structure copolymer " structure, it is contemplated that oxidant is successfully wrapped up by polymer, is realized Microencapsulation.
Fig. 2 is the release time of oxidant microcapsules in embodiment 1 with concentration of lye variation diagram.As seen from Figure 2：It is prepared Oxidant microcapsules, delivery mode be timing concentrate release and its release time can by adjust lye concentration come smart Really regulation.
Embodiment 2：
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, oleic acid, lauryl alcohol, acetic acid second Ester accounts for 0.9%, 0.6%, the 75.93% of the total amount that feeds intake respectively, is stirred to react 5~6min：
(2) potassium peroxydisulfate, epoxy resin, polyamide and the silica of certain mass ratio, ammonium persulfate, ring is added Oxygen resin, polyamide, silica account for 8%, 8%, 5%, the 0.3% of the total amount that feeds intake respectively, and the reaction was continued 40~ 50min；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, ethylenediamine, ethyl alcohol account for the total amount that feeds intake respectively 0.07%, 1.2%, continue to be stirred to react 12~14h, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
Embodiment 3：
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, oleic acid, lauryl alcohol, acetic acid second Ester accounts for 0.6%, 0.5%, the 81.75% of the total amount that feeds intake respectively, is stirred to react 5~6min；
(2) chromium trichloride, epoxy resin, polyamide and the silica of certain mass ratio, ammonium persulfate, ring is added Oxygen resin, polyamide, silica account for 6%, 6%, 4%, the 0.1% of the total amount that feeds intake respectively, and the reaction was continued 40~ 50min；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, ethylenediamine, ethyl alcohol account for the total amount that feeds intake respectively 0.05%, 1%, continue to be stirred to react 12~14h, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
Embodiment 4
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, oleic acid, lauryl alcohol, acetic acid second Ester accounts for 0.8%, 0.45%, the 80.59% of the total amount that feeds intake respectively, is stirred to react 5~6min；
(2) sodium dichromate, epoxy resin, polyamide and the silica of certain mass ratio, ammonium persulfate, ring is added Oxygen resin, polyamide, silica account for 7%, 7%, 3%, the 0.2% of the total amount that feeds intake respectively, and the reaction was continued 40~ 50min；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, ethylenediamine, ethyl alcohol account for the total amount that feeds intake respectively 0.06%, 0.9%, continue to be stirred to react 12~14h, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
Embodiment 5
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, oleic acid, lauryl alcohol, acetic acid second Ester accounts for 0.9%, 0.6%, the 81.2% of the total amount that feeds intake respectively, is stirred to react 5~6min；
(2) potassium permanganate, epoxy resin, polyamide and the silica of certain mass ratio, ammonium persulfate, ring is added Oxygen resin, polyamide, silica account for 5%, 7.5%, 3.5%, the 0.15% of the total amount that feeds intake respectively, and the reaction was continued 40~ 50min；
(3) it is slowly added to the ethylenediamine and alcohol mixeding liquid of certain mass ratio, ethylenediamine, ethyl alcohol account for the total amount that feeds intake respectively 0.05%, 1.1%, continue to be stirred to react 12~14h, deionized water and ethyl alcohol are respectively washed twice, and oxidant microcapsules are obtained.
The foregoing examples are merely illustrative of the technical concept and features of the invention, its object is to allow one skilled in the art It cans understand the content of the present invention and implement it accordingly, it is not intended to limit the scope of the present invention.It is all smart according to the present invention The equivalent transformation or modification that refreshing essence is done, should be covered by the protection scope of the present invention.

Claims (2)

1. a kind of preparation method of lye control release type nano oxygen agent microcapsules, it is characterised in that include the following steps：
(1) oleic acid, lauryl alcohol and ethyl acetate of certain mass ratio are weighed in reactor, is stirred to react 5~6min；
(2) oxidant, epoxy resin, polyamide and the silica of certain mass ratio is added, the reaction was continued 40~ 50min；
(3) ethylenediamine and alcohol mixeding liquid of certain mass ratio are slowly added to, continues to be stirred to react 12~14h, deionized water and Ethyl alcohol is respectively washed twice, and oxidant microcapsules are obtained；
The oxidant, oleic acid, lauryl alcohol, epoxy resin, polyamide, silica, ethylenediamine, ethyl alcohol, ethyl acetate 5%~8%, 0.5%~0.9%, 0.4%~0.6%, 5%~8%, 3%~5%, the 0.1% of the total weight that feeds intake is accounted for respectively ~0.3%, 0.04%~0.07%, 0.8%~1.2%, 75.93%~85.16%.
2. the preparation method of lye control release type nano oxygen agent microcapsules according to claim 1, it is characterised in that： The oxidant is one of ammonium persulfate, potassium peroxydisulfate, chromium trichloride, sodium dichromate, potassium bichromate, potassium permanganate.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
CN102533244B (en) * 2010-12-27 2013-10-16 中国石油天然气股份有限公司 Encapsulated sustained-release acid for oil-water well reconstruction and preparation method thereof
CN102690645B (en) * 2012-06-08 2014-07-02 中国海洋石油总公司 Sustained-release gel-breaking type fracturing propping agent and preparation method thereof
CN103361039B (en) * 2013-08-02 2016-06-29 中国石油集团川庆钻探工程有限公司 Formation temperature is utilized to generate the method for blocking that pack-off valve blocks the fluid gel of gas-bearing formation

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US20070298977A1 (en) * 2005-02-02 2007-12-27 Halliburton Energy Services, Inc. Degradable particulate generation and associated methods

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102533244B (en) * 2010-12-27 2013-10-16 中国石油天然气股份有限公司 Encapsulated sustained-release acid for oil-water well reconstruction and preparation method thereof
CN102690645B (en) * 2012-06-08 2014-07-02 中国海洋石油总公司 Sustained-release gel-breaking type fracturing propping agent and preparation method thereof
CN103361039B (en) * 2013-08-02 2016-06-29 中国石油集团川庆钻探工程有限公司 Formation temperature is utilized to generate the method for blocking that pack-off valve blocks the fluid gel of gas-bearing formation

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