CN106000248B - A kind of preparation method of controllable expansion super moisture absorbing resin microcapsules - Google Patents
A kind of preparation method of controllable expansion super moisture absorbing resin microcapsules Download PDFInfo
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- CN106000248B CN106000248B CN201610367600.0A CN201610367600A CN106000248B CN 106000248 B CN106000248 B CN 106000248B CN 201610367600 A CN201610367600 A CN 201610367600A CN 106000248 B CN106000248 B CN 106000248B
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- 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
- B01J13/06—Making microcapsules or microballoons by phase separation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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Abstract
The invention discloses a kind of preparation methods of super moisture absorbing resin microcapsules comprising following steps：It is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether in three-necked flask.Reaction temperature is down to 70 DEG C by the mixed liquor that quantitative isopropanol, ethyl alcohol, butyl titanate and odium stearate composition are then added into flask after being reacted 50 minutes under conditions of 90 DEG C.Successively into flask be added corrresponding quality than Tween 80 and lauryl sodium sulfate, the reaction was continued 1 hour, is slowly added to the mixture of the butyl acrylate containing azodiisobutyronitrile and acrylic acid, and the reaction was continued under conditions of 70 DEG C a period of time, cooling device receives sample.The present invention produces the super moisture absorbing resin microcapsules being prepared.
Description
Technical field
The invention belongs to oil exploitation, technical field of chemistry and chemical engineering, and in particular to a kind of controllable expansion super moisture absorbing resin is micro-
Capsule and preparation method.
Background technology
Super moisture absorbing resin is the functional high molecule material containing strongly hydrophilic group, it can absorb own wt hundred times
The even water of thousands of times of weight, rapid spatial expansion after water suction, and there is very strong water-retaining property, apply pressure, the water of absorption
It also is difficult to be extruded out.The inner molecular structure of super moisture absorbing resin is tridimensional network, becomes certain viscous after water swelling
The gelinite of elasticity has certain intensity, stronger water-retaining property, salt-resistance and stability.
Super moisture absorbing resin is added in drilling fluid and can be used for oil well leak stopping.It not only can be used alone, can also be with
Other plugging materials are used in compounding to control the leakage of drilling fluid.Under external pressure displacement effect, super moisture absorbing resin generates bullet
Property deformation and pierce oil well crack or blowhole, blocking is generated to oil well after squeezing and accumulating, in addition super moisture absorbing resin into
It still will continue to expand after entering drop ply, keep plugged zone more fine and close, to enhance plugging effect, improve the bearing capacity of drop ply.With
Other plugging materials are compared, and super moisture absorbing resin has many advantages, such as that dosage is few, is easily-synthesized, is at low cost, is easy for construction, while it can also
Large range of all kinds of oil well cracks and hole are adapted to, is a kind of preferable New Kind of Plugging Agent of development prospect.
But conventional use of water-absorbing resin, rate of water absorption is too fast, and saturation can be reached in three had minute, to draw
The phenomenon that playing pumping difficulties；Even volume is excessive after some resin water swellings, it is caused to cannot be introduced into oil well drop ply, direct shadow
Ring plugging effect.If in capable of wrapping up super moisture absorbing resin into microcapsules and controlling its rate of release and can efficiently solve above-mentioned ask
Topic.Super moisture absorbing resin microcapsules are pumped to the specified drop ply position of oil well, after a period of time, under the conditions of oil temperature, and micro- glue
Capsule coating material ruptures and releases super moisture absorbing resin, and water-absorbing resin absorbs the water in stratum and expands rapidly, Jin Eryou at this time
Effect blocks oil well drop ply.
Therefore, select suitable preparation method that super moisture absorbing resin is realized microencapsulation, to improve it in oil well leak stopping
The application of aspect has epochmaking actual application value.
Invention content
The technology of the present invention can solve：By the way that super moisture absorbing resin is realized microencapsulation, to realize its water swelling rate
Controllable purpose further increases the oil well of super moisture absorbing resin so that it is used to meet when oil well leak stopping the requirement of Bulking Time
Plugging effect and its application in terms of the leak stopping of oil field.
The technical issues of to solve above-mentioned first aspect, the system of controllable expansion super moisture absorbing resin microcapsules provided by the invention
Preparation Method includes the following steps：
(1) it is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether, be configured to solution A,
(2) by a certain amount of isopropanol, ethyl alcohol, butyl titanate and odium stearate, it is configured to solution B,
(3) mixture of butyl acrylate and acrylic acid, is configured to solution C,
(4) solution B is added in the solution A, stirs evenly and is reacted,
(5) after the completion of waiting for that reaction is fast, it is eventually adding solution C, is stirred for homogeneous reaction for a period of time；
(6) last cooling device receives sample.
Preferably, in the step (4), after being reacted 40-60 minutes under conditions of 80 DEG C -95 DEG C, reaction temperature is dropped
To 65 DEG C -75 DEG C.
Preferably, in the step (5), when being slowly added to solution C the reaction was continued under conditions of 65 DEG C -75 DEG C one section
Between.
Preferably, the reaction raw materials of super moisture absorbing resin microcapsules and weight percent are：Super moisture absorbing resin 3%~8%, ring
Hexane 45%~65%, petroleum ether 15%~25%, isopropanol 1%~2.5%, ethyl alcohol 2%~4%, butyl titanate 1%~
3.5%, odium stearate 1.5%~4%, butyl acrylate 1.5%~4%, acrylic acid 2.5%~6%.
Preferably, 0.5%~1.5% Tween 80,0.5%~1% dodecane are additionally added before the step (5)
Base sodium sulphate.
Preferably, 0.05%~0.1% azodiisobutyronitrile is additionally added in the step (3) solution C.
Preferably, the reaction raw materials of super moisture absorbing resin microcapsules and weight percent are：Super moisture absorbing resin 3%~8%, ring
Hexane 45%~65%, petroleum ether 15%~25%, isopropanol 1%~2.5%, ethyl alcohol 2%~4%, butyl titanate 1%~
3.5%, odium stearate 1.5%~4%, butyl acrylate 1.5%~4%, acrylic acid 2.5%~6%, Tween 80 0.5%~
1.5%, lauryl sodium sulfate 0.5%~1%, azodiisobutyronitrile 0.05%~0.1%.
Preferably, the raw material of super moisture absorbing resin microcapsules and weight percent are：Super moisture absorbing resin 3%, hexamethylene
60.45%, petroleum ether 20%, isopropanol 1.5%, ethyl alcohol 3%, butyl titanate 1.5%, odium stearate 2.5%, butyl acrylate
2%, acrylic acid 4.5%, Tween 80 1%, lauryl sodium sulfate 0.5%, azodiisobutyronitrile 0.05%.
Preferably, the reaction raw materials of super moisture absorbing resin microcapsules and weight percent are：Super moisture absorbing resin 6%, hexamethylene
52.4%, petroleum ether 15%, isopropanol 2.5%, ethyl alcohol 4%, butyl titanate 3.5%, odium stearate 4%, butyl acrylate
4%, acrylic acid 6%, Tween 80 1.5%, lauryl sodium sulfate 1%, azodiisobutyronitrile 0.1%.
The second aspect of the present invention provides a kind of controllable expansion super moisture absorbing resin microcapsules, is prepared by the following method
It arrives：
(1) it is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether, be configured to solution A,
(2) by a certain amount of isopropanol, ethyl alcohol, butyl titanate and odium stearate, it is configured to solution B,
(3) mixture of butyl acrylate and acrylic acid, is configured to solution C,
(4) solution B is added in the solution A, stirs evenly and is reacted,
(5) after the completion of waiting for that reaction is fast, it is eventually adding solution C, is stirred for homogeneous reaction for a period of time；
(6) last cooling device receives sample.
Preferably, the reaction raw materials of controllable expansion super moisture absorbing resin microcapsules and weight percent are：Super moisture absorbing resin 3%
~8%, hexamethylene 45%~65%, petroleum ether 15%~25%, isopropanol 1%~2.5%, ethyl alcohol 2%~4%, metatitanic acid fourth
Ester 1%~3.5%, odium stearate 1.5%~4%, butyl acrylate 1.5%~4%, acrylic acid 2.5%~6%.
The third aspect of the present invention provides a kind of controllable expansion super moisture absorbing resin microcapsules for absorbing liquid, aqueous use
On the way.It is preferred that super moisture absorbing resin microcapsules at 60-80 DEG C absorb it is liquid, aqueous.
In currently preferred technical solution, the preparation method of controllable expansion super moisture absorbing resin microcapsules, including walk as follows
Suddenly：It is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether in three-necked flask.Then it is added into flask
The mixed liquor of quantitative isopropanol, ethyl alcohol, butyl titanate and odium stearate composition, after being reacted 50 minutes under conditions of 90 DEG C,
Reaction temperature is down to 70 DEG C.Be added successively into flask corrresponding quality than Tween 80 and lauryl sodium sulfate, continue anti-
Answer 1 hour, be slowly added to the mixture of the butyl acrylate containing azodiisobutyronitrile and acrylic acid, under conditions of 70 DEG C after
Continuous reaction a period of time, cooling device receive sample.
In the present invention, technical name " super moisture absorbing resin ", including the ionic in the prior art classified according to functional group,
Nonionic；According to the starch of raw material sources, cellulose family and synthesis class；The hydrophilic monomer divided according to hydrophily is directly poly-
Conjunction, the hydrophilic monomer grafting of hydrophobic monomer carboxy methylation, hydrophobic polymer, itrile group, hydrolysis of ester group class；Further include that ontology is poly-
The super moisture absorbing resin that the methods of conjunction, polymerisation in solution, inverse suspension polymerization and inverse emulsion polymerization are prepared, also draws including ultrasound
The super moisture absorbing resin that the methods of hair, ultraviolet light-initiated, microwave radiation initiation are prepared.
The purpose and meaning of the rate of charge：It is prepared when the additive amount of above-mentioned drug is in range defined above
Super moisture absorbing resin encapsulation rate is higher (up to 96%), while the control of its production cost is in relatively low range.
The controllable expansion super moisture absorbing resin microcapsules that the present invention is prepared can be on defined period, usual 10 minutes left sides
Right implosion simultaneously releases super moisture absorbing resin, to efficiently control the Bulking Time of super moisture absorbing resin.
Description of the drawings
Fig. 1 (a) is that the digital photograph figure after 2 minutes in 25 DEG C of water is added in super moisture absorbing resin.
Fig. 1 (b) is that the digital photograph figure after 2 minutes in 25 DEG C of water is added in super moisture absorbing resin microcapsules.
Fig. 1 (c) is the digital photograph figure in super moisture absorbing resin 25 DEG C of water of addition after ten minutes.
Fig. 1 (d) is the digital photograph figure in super moisture absorbing resin microcapsules 25 DEG C of water of addition after ten minutes.
Fig. 2 (a) is that the digital photograph figure after 2 minutes in 70 DEG C of water is added in super moisture absorbing resin microcapsules.
Fig. 2 (b) is the digital photograph figure in super moisture absorbing resin microcapsules 70 DEG C of water of addition after ten minutes.
Specific implementation mode
The following examples are the present invention to be expanded on further, but present disclosure is without being limited thereto.Present invention explanation
Embodiment in book is only used for that the present invention will be described, does not play restriction effect to protection scope of the present invention.This
The protection domain of invention is only defined by the claims, and those skilled in the art are in embodiment disclosed by the invention on the basis of institute
Any omission, replacement or the modification made fall within protection scope of the present invention.
1. controllable expansion super moisture absorbing resin microcapsule preparation method of embodiment
Reaction raw materials and percentage are super moisture absorbing resin 3%, petroleum ether 20%, isopropanol 1.5%, ethyl alcohol 3%, metatitanic acid fourth
Ester 1.5%, odium stearate 2.5%, Tween 80 1%, lauryl sodium sulfate 0.5%, azodiisobutyronitrile 0.05%, propylene
Acid butyl ester 2%, acrylic acid 4.5%, remaining is hexamethylene, adds up to 100%.Each component accounts for the total weight that feeds intake in its concrete composition
Percentage (100%).
It is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether in three-necked flask.Then to flask
The middle mixed liquor that quantitative isopropanol, ethyl alcohol, butyl titanate and odium stearate composition is added, reacts 50 points under conditions of 90 DEG C
Reaction temperature is down to 70 DEG C by Zhong Hou.Successively into flask be added corrresponding quality than Tween 80 and lauryl sodium sulfate, after
Continuous reaction 1 hour, is slowly added to the mixture of the butyl acrylate containing azodiisobutyronitrile and acrylic acid, in 70 DEG C of condition
The reaction was continued down a period of time, and cooling device receives sample.
2. controllable expansion super moisture absorbing resin microcapsule preparation method of embodiment
Reaction raw materials and percentage are：Super moisture absorbing resin 4.5%, petroleum ether 15%, isopropanol 1.5%, ethyl alcohol 2.5%,
Butyl titanate 2%, odium stearate 2.5%, Tween 80 1.5%, lauryl sodium sulfate 0.5%, azodiisobutyronitrile
0.08%, butyl acrylate 3%, acrylic acid 3.5%, remaining is hexamethylene, adds up to 100%.
Reaction step method is same as above.
3. controllable expansion super moisture absorbing resin microcapsule preparation method of embodiment
Reaction raw materials and percentage are：Super moisture absorbing resin 8%, petroleum ether 10%, isopropanol 1.5%, ethyl alcohol 4%, metatitanic acid
Butyl ester 2%, odium stearate 4%, Tween 80 1.5%, lauryl sodium sulfate 0.5%, azodiisobutyronitrile 0.1%, acrylic acid
Butyl ester 4%, acrylic acid 5%, remaining is hexamethylene, adds up to 100%.
Reaction step method is same as above.
Embodiment 4：Controllable expansion super moisture absorbing resin microcapsule preparation method
Reaction raw materials and percentage are：Super moisture absorbing resin 5%, petroleum ether 25%, isopropanol 2.5%, ethyl alcohol 4%, metatitanic acid
Butyl ester 2.5%, odium stearate 3.5%, Tween 80 1%, lauryl sodium sulfate 1%, azodiisobutyronitrile 0.07%, propylene
Acid butyl ester 3.5%, acrylic acid 5%, remaining is hexamethylene, adds up to 100%.
Reaction step method is same as above.
Embodiment 5：Controllable expansion super moisture absorbing resin microcapsule preparation method
Reaction raw materials and percentage are：Super moisture absorbing resin 6%, petroleum ether 15%, isopropanol 2.5%, ethyl alcohol 4%, metatitanic acid
Butyl ester 3.5%, odium stearate 4%, Tween 80 1.5%, lauryl sodium sulfate 1%, azodiisobutyronitrile 0.1%, acrylic acid
Butyl ester 4%, acrylic acid 6%, remaining is hexamethylene, adds up to 100%.
Reaction step method is same as above.
Embodiment 6：Control experiment
Controllable expansion super moisture absorbing resin microcapsules and each 3g of super moisture absorbing resin prepared by embodiment 1 are chosen, are added to 25 DEG C
In water, Observe and measure is carried out in 2 minutes, 10 minutes points；The micro- glue of controllable expansion super moisture absorbing resin prepared by another Example 1
Capsule 3g is added in 70 DEG C of water, and Observe and measure is carried out in 2 minutes, 10 minutes points.As a result as shown in Fig. 1 (a) -1 (d), such as
Shown in Fig. 2 (a), 2 (b).
From Fig. 1 (a)：Super moisture absorbing resin is added into water rear rapid water swelling and is settled down to beaker bottom.From Fig. 1
(b) visible：Super moisture absorbing resin microcapsules are no after being added into water to occur apparent water swelling phenomenon, while the microcapsules float
It bubbles through the water column.
From Fig. 1 (c)：Super moisture absorbing resin is added into water water swelling after ten minutes to being saturated, and is in gel.From figure
1 (d) is visible：Super moisture absorbing resin microcapsules are added into water after ten minutes also without apparent water swelling phenomenon occurs (only
There is the water swelling of minute quantity sample and be settled down to beaker bottom).
From Fig. 2 (a)：Super moisture absorbing resin microcapsules are added into 70 DEG C of water after 2 minutes, and sample starts expansion and becomes larger,
And all it is settled down to beaker bottom.
From Fig. 2 (b)：Super moisture absorbing resin microcapsules are added into 70 DEG C of water after ten minutes, and sample water swelling is to full
With, be in gel.
Specific response data is as follows：
According to above control experiment, it is known that the super moisture absorbing resin microcapsules that the present invention is prepared under the conditions of 25 DEG C not
Water swelling occurs, and sample starts water swelling under the conditions of 70 DEG C, after 2 minutes, and sample water swelling is to full after ten minutes
With, be in gel.Illustrate that super moisture absorbing resin microcapsules prepared by the present invention have certain temperature-responsive, only works as microcapsules
Within the scope of preferred temperature when (60~80 DEG C), microcapsules shell material can just rupture and release super moisture absorbing resin, at this time superabsorbent
The rapid water swelling of water-resin simultaneously reaches saturation, and then effectively blocks oil well drop ply.
The foregoing examples are merely illustrative of the technical concept and features of the invention, its object is to allow the person skilled in the art to be
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 (7)
1. the preparation method of controllable expansion super moisture absorbing resin microcapsules, feature include the following steps：
（1）It is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether, be configured to solution A,
（2）By a certain amount of isopropanol, ethyl alcohol, butyl titanate and odium stearate, it is configured to solution B,
（3）The mixture of butyl acrylate and acrylic acid, is configured to solution C,
（4）The solution B is added in the solution A, stirs evenly and reacted, under conditions of 80 DEG C -95 DEG C
After reaction 40-60 minutes, reaction temperature is down to 65 DEG C -75 DEG C;
（5）After the completion of waiting for that reaction is fast, it is slowly added to solution C the reaction was continued under conditions of 65 DEG C -75 DEG C a period of time；
（6）Last cooling device receives sample;
The raw material and weight percent of super moisture absorbing resin microcapsules be：Super moisture absorbing resin 3% ~ 8%, hexamethylene 45% ~ 65%, petroleum ether
15% ~ 25%, isopropanol 1% ~ 2.5%, ethyl alcohol 2% ~ 4%, butyl titanate 1% ~ 3.5%, odium stearate 1.5% ~ 4%, butyl acrylate
1.5% ~ 4%, acrylic acid 2.5% ~ 6%.
2. the preparation method of controllable expansion super moisture absorbing resin microcapsules according to claim 1, which is characterized in that described
Step（5）It is additionally added 0.5% ~ 1.5% Tween 80,0.5% ~ 1% lauryl sodium sulfate before.
3. the preparation method of controllable expansion super moisture absorbing resin microcapsules according to claim 1, which is characterized in that described
Step（3）0.05% ~ 0.1% azodiisobutyronitrile is additionally added in solution C.
4. a kind of controllable expansion super moisture absorbing resin microcapsules, which is characterized in that it is prepared by the following method：
（1）It is accurate weigh certain mass than super moisture absorbing resin, hexamethylene and petroleum ether, be configured to solution A,
（2）By a certain amount of isopropanol, ethyl alcohol, butyl titanate and odium stearate, it is configured to solution B,
（3）The mixture of butyl acrylate and acrylic acid, is configured to solution C,
（4）The solution B is added in the solution A, stirs evenly and reacted,
（5）After the completion of waiting for that reaction is fast, it is eventually adding solution C, is stirred for homogeneous reaction for a period of time；
（6）Last cooling device receives sample.
5. controllable expansion super moisture absorbing resin microcapsules according to claim 4, which is characterized in that super moisture absorbing resin microcapsules
Reaction raw materials and weight percent be：Super moisture absorbing resin 3% ~ 8%, hexamethylene 45% ~ 65%, petroleum ether 15% ~ 25%, isopropanol 1%
~ 2.5%, ethyl alcohol 2% ~ 4%, butyl titanate 1% ~ 3.5%, odium stearate 1.5% ~ 4%, butyl acrylate 1.5% ~ 4%, acrylic acid 2.5% ~
6%。
6. the controllable expansion super moisture absorbing resin microcapsules described in a kind of claim 4 are for absorbing liquid, aqueous purposes.
7. purposes according to claim 6, which is characterized in that the controllable expansion super moisture absorbing resin microcapsules are in 60-80
DEG C absorb liquid, aqueous.
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|---|---|---|---|---|
| CN1486782A (en) * | 2003-01-16 | 2004-04-07 | 大连理工大学 | High-hydroscopicity polymer resin microcapsule and its production process |
| CN103554331A (en) * | 2013-11-05 | 2014-02-05 | 中海油能源发展股份有限公司惠州石化分公司 | Method for preparing polyacrylic acid high-water-absorptivity resin microspheres by reversed phase suspension polymerization |
| CN104448102A (en) * | 2014-11-27 | 2015-03-25 | 成都锦汇科技有限公司 | Method for preparing super absorbent resin microspheres |
| WO2016073004A1 (en) * | 2014-11-07 | 2016-05-12 | Halliburton Energy Services, Inc. | Fluid loss additive package for shallow well drilling fluids |
-
2016
- 2016-05-30 CN CN201610367600.0A patent/CN106000248B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1486782A (en) * | 2003-01-16 | 2004-04-07 | 大连理工大学 | High-hydroscopicity polymer resin microcapsule and its production process |
| CN103554331A (en) * | 2013-11-05 | 2014-02-05 | 中海油能源发展股份有限公司惠州石化分公司 | Method for preparing polyacrylic acid high-water-absorptivity resin microspheres by reversed phase suspension polymerization |
| WO2016073004A1 (en) * | 2014-11-07 | 2016-05-12 | Halliburton Energy Services, Inc. | Fluid loss additive package for shallow well drilling fluids |
| CN104448102A (en) * | 2014-11-27 | 2015-03-25 | 成都锦汇科技有限公司 | Method for preparing super absorbent resin microspheres |
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