CN102989395A - Process for preparing liquid microcapsule gel breaker based on drying temperature control - Google Patents
Process for preparing liquid microcapsule gel breaker based on drying temperature control Download PDFInfo
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- CN102989395A CN102989395A CN 201110290403 CN201110290403A CN102989395A CN 102989395 A CN102989395 A CN 102989395A CN 201110290403 CN201110290403 CN 201110290403 CN 201110290403 A CN201110290403 A CN 201110290403A CN 102989395 A CN102989395 A CN 102989395A
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Abstract
The invention discloses a process for preparing a liquid microcapsule gel breaker based on drying temperature control. The process for preparing the liquid microcapsule gel breaker based on the reaction temperature control mainly comprises the following five stages of: preparing a wall material solution, emulsifying a core material, encapsulating, curing microcapsules, and drying the microcapsules, wherein the reaction temperature is controlled to be 70 to 80 DEG C in the preparation process. The drying temperature in the preparation process is controlled, so that the liquid microcapsule gel breaker prepared by using the method is excellent in performances, simple in production process and high in production efficiency, and the production cost is greatly reduced.
Description
Technical field
The present invention relates to a kind of liquid microcapsule gel breaker preparation technology based on the control baking temperature.
Background technology
Microcapsules are actually some little particles, and these little particles wrap the material that another kind is referred to as core by a kind of material that is referred to as the wall material and formed.On this basis, also have the microcapsules of some specific types, such as checking microcapsules, multiple wall microcapsules and occurring matrix type microcapsules etc.Enveloped is the two-phase of separating with cyst wall, and this is the feature of microcapsules.Microcapsules not only can the encapsulated solid powder, also can the enclosed liquid material.As adopting special preparation method, microcapsules can also be sealed gas.In addition.Hydrophobic material and water wetted material all can be encapsulated in the microcapsules.
The technical research of microcapsules probably starts from the thirties in last century, and being attended by the most momentous results is in the fifties.In the developing history process of microcapsules technology, the U.S. maintains the leading position to its research always, and Japan has also caught up with in 60～seventies gradually.China is starting late aspect the research microcapsules technology, but all has practical application and more deep research at aspects such as medicine, agricultural chemicals, cosmetics, food.The Microcapsules Size of initial preparation is called micron-sized microcapsules between 5～2000 microns.Along with the development of microcapsules technology, the particle diameter of the microcapsules of preparation can reach between 1～1000 nanometer less than 1 micron, often is called as Nano capsule.Along with the continuous progress of microcapsules technology, microcapsules will bring larger benefit to the mankind.
Microcapsules can have multiple sorting technique by the different criteria for classifying.This paper is different according to the shell material of microcapsules and core material performance, microcapsules mainly can be divided into following several types by purposes:
1. slow-release type microcapsule
The wall of these microcapsules is equivalent to a pellicle, allows core material to see through under certain condition, to prolong the action time of core material.Difference according to wall material source can be divided into natural polymer slow-release material (gelatin and carboxymethyl cellulose) and synthetic high polymer slow-release material.And for the synthetic high polymer slow-release material, different by its biodegradability, can be divided into again Biodegradable and non-biodegradation type two large classes.
2. pressure sensitive microcapsules
This kind encapsulation the core material of some question responses, when pressure-acting after microcapsules surpass certain limit, the microcapsules cyst wall breaks and flows out core material, because the variation of external environment, core material produces chemical reaction and shows color or other phenomenon occurs.
3. thermosensitive type microcapsules
Make cyst wall softening or break and discharge core material because temperature raises, be core material because the change generation molecular rearrangement of temperature or geometrical isomerism and colorific variation sometimes.
4. Photosensitive microcapsules
After cyst wall broke, photoactive substance in the core selected to absorb the light of specific wavelength, sensitization or molecular energy transition occur and produces corresponding reaction or variation.
5. intumescent microcapsules
Cyst wall is thermoplastic high-air-tightness material, and core is volatile low boiling point solvent, be higher than the boiling point of solvent when temperature after, solvent evaporation and make microcapsule expansion, microcapsules are still kept the state before expanding after the cooling.
General any physical form that has wrapped up the similar small containers of certain material all can be referred to as microcapsules, so except above-mentioned 5 types, micro-emulsion, liposome and non-ionic surface active agent microvesicle also can be described as microcapsules.
Burnham has just reported that as far back as the beginning of the eighties preparation microcapsule degelling agent can reach the purpose that postpones broken glue.After this, Nolte and Wal les have also reported respectively capsule breaker technology of preparing separately.The end of the eighties, Halliburton and Dowell, the companies such as Schlumberger have all carried out desk research and the field work of capsule Delayed Release Breaker in succession.Since using at the scene first capsule breaker from the fourth quarter in 1989, postpone broken glue technology and once comprising California, New Mexico, use in the hundreds of mouth Oil/gas Well in the areas such as Rashid Sidek Sa Si, compare with the conventional break agent, bleed rate increases, and needs the well of pumping greatly to reduce, and cumulative production and initil output all obviously increase.
After microcapsules form, need to carry out drying to microcapsules and process, obtain the solid microscapsule powder, be convenient to store transportation.Baking temperature has certain impact to particle diameter and the intensity of microcapsules.When drying, temperature raises, the product moisture evaporation, and particle diameter must reduce.Temperature is too low, and deficiency is so that moisture evaporates, and product strength reduces, and stores the caking that easily sticks together.Temperature is too high, and the wall material melts, and core easily discharges.It is minimum that suitable baking temperature will guarantee that namely the moisture of product is reduced to, and also will make product keep good shape.
Summary of the invention
Purpose of the present invention is in order to overcome the deficiencies in the prior art and defective, a kind of liquid microcapsule gel breaker preparation technology based on the control baking temperature is provided, this preparation technology is by the baking temperature in the control preparation process, thereby the liquid microcapsule gel breaker properties for preparing is excellent, and production technology is simple, production efficiency is high, greatly reduces production cost.
Purpose of the present invention is achieved through the following technical solutions: the liquid microcapsule gel breaker preparation technology based on the control baking temperature may further comprise the steps:
(a) preparation of wall material solution: take by weighing a certain amount of gelatin and Arabic gum powder, gelatin is soaked swelling after, heating is stirred and to be made its dissolving, and at a certain temperature insulation, and is for subsequent use; Get a certain amount of distilled water and put in the small beaker, add the Arabic gum powder, heating is stirred gently and is made its dissolving, and insulation is for subsequent use at a certain temperature, and with the wall material solution of above-mentioned two kinds of solution mixing systems, and the wall material concentration in the control wall material solution is 1.0%～4.0%;
(b) emulsification of core: get the core of aequum, drip an amount of emulsifying agent, the vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, puts in the water bath with thermostatic control, and mechanical agitation emulsification certain hour,, namely get emulsion;
(c) formation of microcapsules: regulate mechanical agitation speed and bath temperature, under constantly stirring, slowly drip acetum in mixed liquor, the pH value of conditioned reaction system, system viscosity will increase this moment, can observe the formation of microcapsules at microscopically;
(d) curing of microcapsules: the beaker that will contain microcapsules liquid takes off in water-bath, does not stop to stir, and naturally cooling adds ice cube, continue to stir, the adding curing agent is an amount of, transfers its pH with NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the micro-capsule sedimentation;
(e) drying of microcapsules: after the micro-capsule sedimentation fully, the supernatant that inclines filters (or drying), and micro-capsule washs with distilled water, drains, and places insulating box dry, and the baking temperature of control insulating box is 70 ℃～80 ℃, namely gets product.
In the described step (a), gelatin is with an amount of distilled water immersion swelling.
In the described step (a), be heated to 50 ℃.
In the described step (a), holding temperature is 40 ℃.
In the described step (a), be heated to 80 ℃.
In the described step (a), holding temperature is 60 ℃.
In the described step (d), treat to add when temperature is 32～35 ℃ ice cube.
In the described step (e), the baking temperature of insulating box is 80 ℃.
In sum, the invention has the beneficial effects as follows: by the baking temperature in the control preparation process, thereby the liquid microcapsule gel breaker properties for preparing is excellent, and production technology is simple, and production efficiency is high, greatly reduces production cost.
The specific embodiment
Below in conjunction with embodiment, to the detailed description further of the present invention's do, but embodiments of the present invention are not limited to this.
Embodiment:
The present invention relates to the liquid microcapsule gel breaker preparation technology based on the control baking temperature, may further comprise the steps:
(a) preparation of wall material solution: take by weighing a certain amount of gelatin and Arabic gum powder, with gelatin with an amount of distilled water immersion swelling after, heating is stirred and to be made its dissolving, and 40 ℃ of lower insulations, and is for subsequent use; Get a certain amount of distilled water and put in the small beaker, add the Arabic gum powder, be heated to 80 ℃, stir gently and make its dissolving, for subsequent use 60 ℃ of lower insulations, above-mentioned two kinds of solution are mixed, namely get wall material solution;
(b) emulsification of core: get the core of aequum, drip an amount of emulsifying agent, the vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, puts in the water bath with thermostatic control, mechanical agitation emulsification a period of time, namely gets emulsion;
(c) formation of microcapsules: regulate mechanical agitation speed and bath temperature, under constantly stirring, slowly drip 10% acetum in mixed liquor, the pH value of conditioned reaction system, system viscosity will increase this moment, can observe the formation of microcapsules at microscopically;
(d) curing of microcapsules: the beaker that will contain microcapsules liquid takes off in water-bath, do not stop to stir, naturally cooling is treated to add ice cube when temperature is 32～35 ℃, and continuing to be stirred to temperature is below 10 ℃, it is an amount of to add curing agent, stir a period of time, transfer its pH with 20%NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leaves standstill and treat the micro-capsule sedimentation;
(e) drying of microcapsules: after the micro-capsule sedimentation fully, the supernatant that inclines filters (or drying), and micro-capsule washs with distilled water, drains, and places insulating box dry, namely gets product.
Test has been investigated different curing agent kinds to the impact of properties of product, and the present invention tests: keep other conditions constant, change baking temperature, prepare several groups of different products, and the difference test performance, the result is as shown in the table:
Can find out that from upper table result baking temperature is not very large to the grain diameter influence of microcapsules, the rising of temperature, particle diameter has by a small margin decline.Reason is the loss of moisture, causes capsule to shrink, and particle diameter diminishes.
Along with the rising of baking temperature, the release rate of microcapsules reduces, and when temperature was elevated to 90 ℃, caking sticked together.
Reason is along with the rising of temperature, and moisture reduces, and particle intensity increases, and release rate reduces; When being elevated to 80 ℃, the release rate of microcapsules is minimum, and keeps good sphericity.Temperature increases again, and polymer film may soften, and sticks together.
Therefore, selecting the baking temperature of microcapsules is 80 ℃.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction, and any simple modification, the equivalent variations on every foundation technical spirit of the present invention above embodiment done all fall within protection scope of the present invention.
Claims (8)
1. based on the liquid microcapsule gel breaker preparation technology of control baking temperature, it is characterized in that, may further comprise the steps:
(a) preparation of wall material solution: take by weighing a certain amount of gelatin and Arabic gum powder, gelatin is soaked swelling after, heating is stirred and to be made its dissolving, and at a certain temperature insulation, and is for subsequent use; Get a certain amount of distilled water and put in the small beaker, add the Arabic gum powder, heating is stirred gently and is made its dissolving, and insulation is for subsequent use at a certain temperature, and with the wall material solution of above-mentioned two kinds of solution mixing systems, and the wall material concentration in the control wall material solution is 1.0%～4.0%;
(b) emulsification of core: get the core of aequum, drip an amount of emulsifying agent, the vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, puts in the water bath with thermostatic control, and mechanical agitation emulsification certain hour,, namely get emulsion;
(c) formation of microcapsules: regulate mechanical agitation speed and bath temperature, under constantly stirring, slowly drip acetum in mixed liquor, the pH value of conditioned reaction system, system viscosity will increase this moment, can observe the formation of microcapsules at microscopically;
(d) curing of microcapsules: the beaker that will contain microcapsules liquid takes off in water-bath, does not stop to stir, and naturally cooling adds ice cube, continue to stir, the adding curing agent is an amount of, transfers its pH with NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the micro-capsule sedimentation;
(e) drying of microcapsules: after the micro-capsule sedimentation fully, the supernatant that inclines filters (or drying), and micro-capsule washs with distilled water, drains, and places insulating box dry, and the baking temperature of control insulating box is 70 ℃～80 ℃, namely gets product.
2. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that, in the described step (a), gelatin is with an amount of distilled water immersion swelling.
3. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that, in the described step (a), is heated to 50 ℃.
4. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that in the described step (a), holding temperature is 40 ℃.
5. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that, in the described step (a), is heated to 80 ℃.
6. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that in the described step (a), holding temperature is 60 ℃.
7. the liquid microcapsule gel breaker preparation technology based on the control baking temperature according to claim 1 is characterized in that, in the described step (d), treats to add when temperature is 32～35 ℃ ice cube.
8. each described liquid microcapsule gel breaker preparation technology based on the control baking temperature is characterized in that in the described step (e), the baking temperature of insulating box is 80 ℃ according to claim 1～7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103627246A (en) * | 2013-12-16 | 2014-03-12 | 北京印刷学院 | Temperature-control microcapsule type drying agent as well as preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103627246A (en) * | 2013-12-16 | 2014-03-12 | 北京印刷学院 | Temperature-control microcapsule type drying agent as well as preparation method and application thereof |
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Application publication date: 20130327 |