CN102989389A - Preparation technology of liquid microcapsule gel breaker by controlling ratio of core to wall - Google Patents
Preparation technology of liquid microcapsule gel breaker by controlling ratio of core to wall Download PDFInfo
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- CN102989389A CN102989389A CN 201110290254 CN201110290254A CN102989389A CN 102989389 A CN102989389 A CN 102989389A CN 201110290254 CN201110290254 CN 201110290254 CN 201110290254 A CN201110290254 A CN 201110290254A CN 102989389 A CN102989389 A CN 102989389A
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Abstract
The invention discloses a preparation technology of a liquid microcapsule gel breaker by controlling a ratio of core to wall. The preparation technology mainly comprises five stages, namely preparation of a wall material solution, emulsification of a core material, encapsulation, microcapsule solidification and microcapsule drying; in the preparation process, the ratio of core to wall is controlled in the range of 3:1-5:1. The prepared liquid microcapsule gel breaker has excellent various performances by controlling the ratio of core to wall. The production technology is simple, production efficiency is high and and production cost is reduced greatly.
Description
Technical field
The present invention relates to a kind of liquid microcapsule gel breaker preparation technology who controls core wall ratio.
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 Walles 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.
Core wall rate of charge has a great impact the performance of microcapsules.For some occasions, as coating dyestuff, wish that core can be coated in the wall material for a long time, the compactness of microcapsules is had relatively high expectations, so just should reduce core wall rate of charge, core as far as possible fully is wrapped by; And other occasions such as coating medicine, essence, wish that then microcapsules have slow-release function, at this moment just should improve core wall rate of charge.In addition, the reduction of core wall ratio can improve the bearing capacity of microcapsules.Microcapsule degelling agent for atoleine, on the one hand, we wish that the core content in the capsule is large as much as possible, improve broken glue efficient, this just needs to improve core wall ratio, but excessive core wall ratio can make strength of microcapsules reduce and softgel shell compactness variation, and Release of core material speed is too fast, can make in advance broken glue of fracturing fluid; Therefore suitable core wall is compared to the atoleine microcapsule degelling agent and seems particularly important.
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 who controls core wall ratio is provided, this preparation technology is by the core wall ratio 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 of control core wall ratio 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, vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, and to control core wall ratio be 3: 1～5: 1, 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 adds ice cube, continues to stir, it is an amount of to add curing agent, stir a period of time, transfer its pH with 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.
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 (b), control core wall ratio is 4: 1.
In sum, the invention has the beneficial effects as follows: by the core wall ratio 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 control the liquid microcapsule gel breaker preparation technology of core wall ratio, may further comprise the steps:
(a) preparation of wall material solution: take by weighing a certain amount of gelatin and Arabic gum powder, and the mass ratio of control gelatin-gum arabic is 5: 5～6: 4; 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, vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, and to control core wall ratio be 3: 1～5: 1, 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.
The impact of different core wall comparison properties of product has been investigated in test, and the present invention has done following experiment:
Testing program:
(1) the preparation quality mark is 4.0% gelatin, gumwater, is incubated for subsequent use.
(2) take by weighing atoleine, making respectively core wall ratio is 1: 1,2: 1,3: 1 and 4: 1, take by weighing again Tween80 and Span80 composite emulsifier (HLB=10.0) with respect to core quality 2.0%, the mix and blend dissolving, pour in gelatin, the gumwater, emulsification 7min under 60 ℃ of water-baths, mixing speed 800r/min condition forms stable emulsion.
(3) adjusting rotary speed is to 500r/min, and temperature to 50 ℃ slowly drips 10% acetum, regulates about pH to 4.0, reaction a period of time, core is fully coated by the wall material.
(4) beaker is taken off in water-bath, do not stop to stir, naturally cooling is when treating that temperature is 32～35 ℃, add ice cube, continuing to be stirred to temperature is below 10 ℃, adds formaldehyde, stirring reaction a period of time, transfer its pH to 9.0 with 20%NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the micro-capsule sedimentation.
(5) filter, washing 60 ℃ of lower dryings, namely obtains product.
Five prepared set products are carried out performance test, and the result is as shown in the table:
As seen from the above table, along with the increase of core wall ratio, the target grain size percentage of gained microcapsules is increase tendency.
Because along with the increase of core, under identical emulsification rotating speed and emulsification times, the suffered shearing force of core was not enough to its minute
Fall apart into enough little particle, the core drop can increase thereupon, so capsule particle must become large.But 3-7 also can from table
Find out that core wall ratio is that the target grain size percentage of 1: 1 gained microcapsules is 2: 1 greater than core wall ratio.When reason was that the capsule-core consumption of synthetic microcapsules is less, the wall material increased the average covering amount of drop, and it is large that particle diameter becomes.
Embedding rate changes not quite at the beginning along with the increase of core concentration, illustrates that the core wall is increased to 4: 1 than from 1: 1 under other condition same cases, and the wall material is basically identical to the coating degree of core.Larger 5: 1 place's embedding rate reduction amplitudes, reason may be that core concentration is excessive, and emulsification is thorough not, and some core easily is gathered into large drop, fails to be wrapped by.
Along with the increase of core wall ratio, the release rate of capsule is increase tendency.Because the increase of core causes particle to increase on the one hand, the wall material amount that average packet overlays on particle surface reduces; On the other hand, core increases, identical emulsification condition, and core material particles is larger, and the capsule intensity of formation must reduce, and under identical pressure, release rate will increase.
The intensity of considering microcapsules can improve by curing agent and later stage condition, and the core wall ratio that we select to prepare this microcapsule degelling agent is 4: 1.
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. the liquid microcapsule gel breaker preparation technology of control core wall ratio 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, vibration dissolving mixes with above-mentioned Arabic gum, gelatin solution, and to control core wall ratio be 3: 1～5: 1, 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 adds ice cube, continues to stir, it is an amount of to add curing agent, stir a period of time, transfer its pH with 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.
2. the liquid microcapsule gel breaker preparation technology of control core wall ratio 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 of control core wall ratio 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 of control core wall ratio 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 of control core wall ratio 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 of control core wall ratio 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 of control core wall ratio according to claim 1 is characterized in that, in the described step (d), treats to add when temperature is 32～35 ℃ ice cube.
8. the liquid microcapsule gel breaker preparation technology of each described control core wall ratio is characterized in that according to claim 1～7, and in the described step (b), control core wall ratio is 4: 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499378A (en) * | 2014-11-21 | 2015-04-08 | 东北林业大学 | Method for preparing environment-friendly waterproof fiberboard based on microcapsule |
| CN104722252A (en) * | 2015-02-06 | 2015-06-24 | 宁波高新区零零七工业设计有限公司 | Preparation process for microcapsule |
| CN105647504A (en) * | 2016-01-25 | 2016-06-08 | 西南石油大学 | Microcapsule gel breaker and preparation method thereof |
| CN105670598B (en) * | 2016-01-11 | 2018-12-04 | 西南石油大学 | A kind of preparation method of potassium peroxydisulfate microcapsule degelling agent |
| CN113662247A (en) * | 2021-09-08 | 2021-11-19 | 湖北中烟工业有限责任公司 | Water-exploded bead core liquid and preparation method thereof |
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2011
- 2011-09-14 CN CN 201110290254 patent/CN102989389A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499378A (en) * | 2014-11-21 | 2015-04-08 | 东北林业大学 | Method for preparing environment-friendly waterproof fiberboard based on microcapsule |
| CN104722252A (en) * | 2015-02-06 | 2015-06-24 | 宁波高新区零零七工业设计有限公司 | Preparation process for microcapsule |
| CN105670598B (en) * | 2016-01-11 | 2018-12-04 | 西南石油大学 | A kind of preparation method of potassium peroxydisulfate microcapsule degelling agent |
| CN105647504A (en) * | 2016-01-25 | 2016-06-08 | 西南石油大学 | Microcapsule gel breaker and preparation method thereof |
| CN113662247A (en) * | 2021-09-08 | 2021-11-19 | 湖北中烟工业有限责任公司 | Water-exploded bead core liquid and preparation method thereof |
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Application publication date: 20130327 |