CN102989394A - Novel preparation technology of liquid microcapsule gel breaker - Google Patents
Novel preparation technology of liquid microcapsule gel breaker Download PDFInfo
- Publication number
- CN102989394A CN102989394A CN 201110290297 CN201110290297A CN102989394A CN 102989394 A CN102989394 A CN 102989394A CN 201110290297 CN201110290297 CN 201110290297 CN 201110290297 A CN201110290297 A CN 201110290297A CN 102989394 A CN102989394 A CN 102989394A
- Authority
- CN
- China
- Prior art keywords
- microcapsules
- gel breaker
- novel preparation
- preparation process
- liquid microcapsule
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a novel preparation technology of a liquid microcapsule gel breaker. The novel 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, a Tween60 and Span60 compounded system is used as an emulsifier. The prepared liquid microcapsule gel breaker has excellent various performances by selecting the appropriate emulsifier. 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 novel preparation process of liquid microcapsule gel breaker.
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.
In the process of preparation liquid microcapsule gel breaker, there is very large impact in the kind of emulsifying agent to the performance of the liquid microcapsule gel breaker that comes prepared, and a kind of suitable emulsifying agent of How to choose seems particularly important to preparation liquid microcapsule gel breaker.
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 novel preparation process of liquid microcapsule gel breaker is provided, this preparation technology is by selecting suitable emulsifying agent, 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 novel preparation process of liquid microcapsule gel breaker 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, and emulsifying agent is Tween60 and Span60 compound system, 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 get 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 sum, the invention has the beneficial effects as follows: by selecting suitable emulsifying agent, 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 novel preparation process of liquid microcapsule gel breaker, 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.
Prepare in the process of microcapsules at gelatin and Arabic gum system, play the salt effect effect in order to prevent inorganic salts, making is separated is affected, and in the attentive response system inorganic salt content low.Therefore, when adding emulsifying agent emulsification core, we only consider non-ionic surface active agent.The present invention chooses respectively Tween60, Tween80, Span60 and Span80 and carries out compositely, obtains four groups of HLB values and be 10.0 emulsifier system.Consumption is 2.0% of core quality.Concrete prescription is as shown in the table:
Testing program:
(1) the preparation quality mark is 4.0% gelatin, gumwater, is incubated for subsequent use.
(2) take by weighing atoleine, make core wall ratio maintain 4: 1; Take by weighing respectively again A, B, C, D 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.
The microcapsules that will prepare under different emulsifiers carry out performance test, and the result is as shown in the table:
The prepared properties of product of emulsifier system B are better as can be seen from the above table.Product objective particle diameter percentage and the embedding rate of preparation are all higher.Release rate is lower, illustrates that product strength is larger.Reason is that the emulsifying capacity of system B is moderate, and core is emulsified into suitable particle diameter, and the wall material can well coat drop, so the microcapsules of target grain size are more, embedding rate increases, and release rate is less.
Therefore, the present invention selects emulsifying agent Tween60 and Span60 compound system as the emulsifying agent of preparing product.
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 (7)
1. the novel preparation process of liquid microcapsule gel breaker 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, and emulsifying agent is Tween60 and Span60 compound system, 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 get 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 novel preparation process of liquid microcapsule gel breaker 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 novel preparation process of liquid microcapsule gel breaker according to claim 1 is characterized in that, in the described step (a), is heated to 50 ℃.
4. the novel preparation process of liquid microcapsule gel breaker according to claim 1 is characterized in that, in the described step (a), holding temperature is 40 ℃.
5. the novel preparation process of liquid microcapsule gel breaker according to claim 1 is characterized in that, in the described step (a), is heated to 80 ℃.
6. the novel preparation process of liquid microcapsule gel breaker according to claim 1 is characterized in that, in the described step (a), holding temperature is 60 ℃.
7. the novel preparation process of liquid microcapsule gel breaker according to claim 1 is characterized in that, in the described step (d), treats to add when temperature is 32～35 ℃ ice cube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110290297 CN102989394A (en) | 2011-09-14 | 2011-09-14 | Novel preparation technology of liquid microcapsule gel breaker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110290297 CN102989394A (en) | 2011-09-14 | 2011-09-14 | Novel preparation technology of liquid microcapsule gel breaker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102989394A true CN102989394A (en) | 2013-03-27 |
Family
ID=47918798
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110290297 Pending CN102989394A (en) | 2011-09-14 | 2011-09-14 | Novel preparation technology of liquid microcapsule gel breaker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102989394A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106070275A (en) * | 2016-06-03 | 2016-11-09 | 安徽广信农化股份有限公司 | The method of the pyraclostrobin microcapsule of preparation uniform particle size |
| 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 |
-
2011
- 2011-09-14 CN CN 201110290297 patent/CN102989394A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106070275A (en) * | 2016-06-03 | 2016-11-09 | 安徽广信农化股份有限公司 | The method of the pyraclostrobin microcapsule of preparation uniform particle size |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102989381A (en) | Preparation technology of liquid microcapsule gel breaker by controlling pH value of system | |
| CN102989389A (en) | Preparation technology of liquid microcapsule gel breaker by controlling ratio of core to wall | |
| CN103170289A (en) | Method for preparing microcapsule phase change material by using composite emulsifier | |
| CN102091579A (en) | Preparation process for gel breaker microcapsules | |
| CN101693640A (en) | Slow-release microcapsule fertilizer and manufacture method thereof | |
| CN102676124B (en) | Inorganic hydrous salt phase change energy storage microcapsule and preparation method thereof | |
| WO2008134908A1 (en) | Wax encapsulation | |
| Wei et al. | Preparation and characterization of novel polyamide paraffin MEPCM by interfacial polymerization technique | |
| CN102989383A (en) | Preparation technology of liquid microcapsule gel breaker by controlling emulsifier dosage | |
| CN102550575A (en) | Pyraclostrobin ester microcapsule suspending agent | |
| CN103555280A (en) | Organic phase change thermal storage material and production method thereof | |
| CN102989394A (en) | Novel preparation technology of liquid microcapsule gel breaker | |
| CN111500264A (en) | Preparation method of hexadecanol-silicon dioxide phase change nano microcapsule | |
| CN105076145A (en) | Microcapsule suspending agent containing azoxystrobin and preparation method thereof | |
| CN102989396A (en) | Process for preparing liquid microcapsule gel breaker based on reaction temperature control | |
| CN111117769A (en) | Nanoscale Pickering emulsion essence and preparation method thereof | |
| CN102989386A (en) | Technology for preparing liquid microcapsule gel breaker for controlling gelatin-Arabic gum ratio | |
| CN102989382A (en) | Preparation technology of liquid microcapsule gel breaker by controlling emulsification revolving speed | |
| CN109908846A (en) | A kind of microcapsules and its preparation method and application | |
| CN102989391A (en) | Preparation technology of liquid microcapsule gel breaker by controlling ratio of core to wall | |
| CN102989384A (en) | Process for preparing liquid microcapsule gel breaker based on emulsifying time control | |
| CN102989392A (en) | Process for preparing liquid microcapsule gel breaker based on control on types of curing agents | |
| CN102989395A (en) | Process for preparing liquid microcapsule gel breaker based on drying temperature control | |
| CN102989397A (en) | Preparation process of liquid microcapsule gel breaker for controlling wall material concentration | |
| CN102989388A (en) | Preparation technology of liquid microcapsule gel breaker by controlling emulsification temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130327 |