CN109880016A - Method for continuous preparation of water-in-oil high internal phase emulsion and polymer porous material - Google Patents
Method for continuous preparation of water-in-oil high internal phase emulsion and polymer porous material Download PDFInfo
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Abstract
本发明涉及连续制备油包水型高内相乳液以及聚合物多孔材料的方法。以乳化剂溶于疏水性单体后所得溶液作为油相；以含电解质和引发剂的水溶液作为水相；将油相和水相分别持续加入到双螺杆挤出机中，通过双螺杆剪切作用，让油相和水相充分乳化形成乳液；油相和水相充分乳化形成乳液后，引发剂引发乳液中的疏水性单体，获得具有孔结构，且孔结构形貌可调的聚合物多孔材料。与现有技术相比，本发明方法简单易行，可用于连续生产高内相乳液，并获得具有特殊孔结构多孔材料。
The present invention relates to a method for continuously preparing a water-in-oil type high internal phase emulsion and a polymeric porous material. The solution obtained by dissolving the emulsifier in the hydrophobic monomer is used as the oil phase; the aqueous solution containing the electrolyte and the initiator is used as the water phase; the oil phase and the water phase are continuously added into the twin-screw extruder, and sheared by the twin-screw The oil phase and the water phase are fully emulsified to form an emulsion; after the oil phase and the water phase are fully emulsified to form an emulsion, the initiator initiates the hydrophobic monomer in the emulsion to obtain a polymer with a pore structure and adjustable pore structure and morphology Porous material. Compared with the prior art, the method of the invention is simple and feasible, can be used for continuous production of high internal phase emulsion, and obtains porous materials with special pore structure.
Description
Technical field
The invention belongs to lotion preparation and porous material preparation technical fields, more particularly, to a kind of continuous preparation oil packet
The method of water type High Internal Phase Emulsion and polymer porous material.
Background technique
High Internal Phase Emulsion, that is, disperse phase volume accounts for the lotion that total emulsion volume score is more than or equal to 74.05%.It is wide
It is general to be applied to food, fuel, oil plant recycling, cosmetics and field of porous materials.High Internal Phase Emulsion is usually by accounting for continuous phase 5-
50% nonionic emulsifier is stabilizer.Also there is nanoparticle to stablize the report of High Internal Phase Emulsion recently.High Internal Phase Emulsion is logical
Often under the action of stabilizer, it is prepared by being gradually added dropwise to dispersed phase in the continuous phase in emulsifying.Its emulsifying manner
Including mechanical stirring, magnetic agitation, emulsification pretreatment, ultrasonic emulsification etc..However these emulsifying manner are clearance-type, i.e. lotion is
One kettle, one kettle or one bottle one bottle preparation, be unfavorable for the stabilization of product emulsion performance.So far, continuous large scale preparation lotion has become
For emulsion technology field problem urgently to be resolved.
In recent years, the polymer porous material as made from High Internal Phase Emulsion template is even more because its unique hole is tied
The characteristics such as structure, high porosity and low-density, excite wide spread interest in multiple fields, they act not only as microelectronics work
The bracket of 3D cell culture, the catalyst in synthesis chemistry and reactant etc. in low-k matrix, organizational project in industry
Carrier, be also used as preparing the template of inorganic porous material.During High Internal Phase Emulsion template prepares porous material,
Performance between emulsion intercalation method and product emulsion batch is unified particularly significant.
The stability of High Internal Phase Emulsion is emphasis concerned by people, it is influenced by many factors.So far, lotion phase
The formation for lotion such as component, emulsifier property and dosage, emulsion dispersion phase volume fraction, preparation temperature, electrolyte concentration
And the influence of stability has been reported that more.Surface is studied, in order to stablize High Internal Phase Emulsion, emulsifier allows for quick adsorption
Onto liquid-liquid interface, one layer of firm interfacial film is formed, and can be effectively reduced the interfacial tension of two-phase interface in lotion.Cream
The stabilization of liquid belongs to dynamic stabilization, it is stabilized by the mutually exclusive power between interior phase drop.Have been generally acknowledged that nonionic
Type emulsifier realizes the stabilization of HIPE by the repulsion benefit on spatial position.It is high interior mutually newborn when to prepare stable Water-In-Oil
Liquid generally requires a kind of nonionic emulsifier of low hydrophilic lipophilic balance, such as sorbitol monooleate (Span80, HLB=
4.3) etc..In addition, electrolyte also also plays important role in terms of High Internal Phase Emulsion stability.The presence of electrolyte can be with
The interaction for weakening emulsifier and aqueous solution makes them in water-oil interface to increase the interaction between emulsifier
It arranges more orderly.Therefore water-oil interface film strength can be enhanced in the addition of electrolyte, increases the elasticity modulus of lotion and apparent
Yield stress, and then improve emulsion intercalation method.On the other hand, dissolution of the electrolyte also by reduction aqueous solution in oily phase
Degree improves the stability of High Internal Phase Emulsion so that Ostwald be inhibited to cure effect.Although the research of High Internal Phase Emulsion is more,
But its emulsifying manner is still limited to the production method of the clearance-types such as mechanical stirring, magnetic agitation, emulsification pretreatment, ultrasonic emulsification, no
Conducive to the stabilization of product emulsion performance, therefore, continuous large scale preparation emulsion technology is still to be developed.
Chinese patent CN102838774B discloses a kind of total with styrene, acrylic acid, methyl methacrylate three block
The water-in-oil type High Internal Phase Emulsion of polymers macromolecular stabilizer is presoma, prepares low-density by being freeze-dried this physics mode
The method of polymer porous material.Steps are as follows: styrene, acrylic acid, methyl methacrylate triblock copolymer are added
Into organic solvent, stirring and dissolving forms polymer solution, using the solution as oily phase, by certain density electrolyte aqueous solution
It is slowly added dropwise in oily phase as water phase, is formed under the action of mechanical stirring and only have the stable water-in-oil type of polymer macromolecule
Lotion is directly fixed pattern with liquid nitrogen frozen, then pass through freeze-drying after placing a period of time at room temperature by High Internal Phase Emulsion
Low-density polymeric porous material is formed after place to go water and organic solvent.
Chinese patent CN102838773B discloses a kind of total with styrene, acrylic acid, methyl methacrylate three block
The stable water-in-oil type High Internal Phase Emulsion of polymers nanoparticle be presoma, by be freeze-dried this physics mode prepare it is ultralow
The method of density polymers porous material.Steps are as follows: electrolyte is added to styrene, acrylic acid, methyl methacrylate
In triblock copolymer nanoparticle aqueous dispersions, it is used as water phase after matter stirring and dissolving to be electrolysed, is then poured slowly into water phase
In oily phase, water-in-oil type High Internal Phase Emulsion is formed under the action of magnetic agitation.Place one section at room temperature to High Internal Phase Emulsion
After time, it is freeze-dried to form low-density polymeric porous material.
Chinese patent CN102391416A discloses one kind in inorganic nano-particle titanium dioxide stabilised oil-in-water height
Phase emulsion, and the method that hydrophilic polymer porous material is obtained as matrix polymerization using this lotion.Steps are as follows: by water-soluble mono
Body, water-soluble cross-linker, electrolyte, initiator are added in the aqueous dispersions of nano-titanium dioxide, and stirring and dissolving is then dripped again
Hydrophobic organic solvent is added, stirring forms emulsion oil-in-water.Heating causes monomer reaction in lotion and obtains hydrophilic polymer
Object porous material.
Above-mentioned three patents be all study before present inventor about the preparation of water-in-oil type High Internal Phase Emulsion and
The related patents of polymer porous material preparation, emulsifying manner of above-mentioned three patents are still limited to the production method of clearance-type, no
It can continuous large scale preparation lotion.
On the other hand, from nineteen thirty-five, Italian Roberto Colombo and Carlo Pasqutti is developed respectively first
Out in the same direction and counter rotation twin screw extruder after, by more than 80 years continuously improve and it is perfect, double screw extruder has obtained considerable
Development, be widely used at present Polymer Processing industry and other industry.Although twin-screw extrusion is in Polymer Processing
Be used widely with modified field, but its in the application of lotion preparation field, there is not been reported.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of continuous preparation oil packets
The method of water type High Internal Phase Emulsion and polymer porous material.
The present invention realizes continuous preparation and the polyalcohol stephanoporate of water-in-oil type High Internal Phase Emulsion using double screw extruder
The continuous preparation of material.
The purpose of the present invention can be achieved through the following technical solutions:
Present invention firstly provides a kind of methods that continuous extrusion prepares water-in-oil type High Internal Phase Emulsion, comprising the following steps:
Acquired solution is as oily phase after being dissolved in hydrophobic monomer using emulsifier；
Using the aqueous solution containing electrolyte as water phase；
It is mutually continuously added into oily in double screw extruder feed opening with water phase, by twin-screw shear action, allows respectively
Water phase is mutually sufficiently mixed with oil, is emulsified, can be obtained water-in-oil type High Internal Phase Emulsion in discharge outlet.
Further, the emulsifier is selected from one of following substance or a variety of: Span80, Span60, polyglycereol alkene
Base succinate or HypermerT96.
Further, the hydrophobic monomer is selected from one of following substance or a variety of: styrene, divinylbenzene,
2-Hydroxyethyl methacrylate, 2-EHA, 2-Ethylhexyl Methacrylate, lauryl acrylate, acrylic acid
Tetradecane base ester, lauryl methacrylate, butyl acrylate, methacrylic acid tetradecane base ester, Glycidyl methacrylate
Glyceride or ethylene glycol dimethacrylate.
Further, the electrolyte is selected from one or both of sodium chloride or calcium chloride.
Further, mass fraction of the emulsifier in oily phase is 5%~30%.
Further, mass fraction of the electrolyte in water phase is 0.5%~3%.
Further, the oil is mutually continuously added into twin-screw respectively and squeezes with the ratio of water phase 1:40~1:3 by volume
Out in machine.
Further, the screw speed of the double screw extruder is 50~350 rpms, and oil is mutually and water phase is in double spiral shells
Temperature in bar extruder is controlled at 20~50 DEG C, and preferably 30~40 DEG C.
Further, initiator is also contained in the water phase, the initiator is in potassium peroxydisulfate or ammonium persulfate
One or two, the initiator amount are the 1%~3% of hydrophobic monomer quality.
In addition the purpose of initiator is, so that containing initiator in last water-in-oil type High Internal Phase Emulsion, exist in this way
Under suitable initiation conditions, the hydrophobic monomer in initiator initiation lotion can use, and then can obtain with pore structure,
And the adjustable polymer porous material of pore structure.
The present invention also provides a kind of preparation methods of polymer porous material, comprising the following steps:
Acquired solution is as oily phase after being dissolved in hydrophobic monomer using emulsifier；
Using the aqueous solution containing electrolyte and initiator as water phase；
It is mutually continuously added into oily in double screw extruder feed opening with water phase, by twin-screw shear action, allows respectively
Water phase is mutually sufficiently mixed with oil, is emulsified, can be obtained water-in-oil type High Internal Phase Emulsion in discharge outlet；
Oily initiator causes the hydrophobic monomer in lotion mutually and after the fully emulsified formation lotion of water phase, and obtaining has hole
Structure, and the adjustable polymer porous material of pore structure.
Further, the initiator is selected from one or both of potassium peroxydisulfate or ammonium persulfate, and the initiator is used
Amount is the 1%~3% of hydrophobic monomer quality.
Further, initiator, which causes the condition of the hydrophobic monomer acquisition polymer porous material in lotion, is: by institute
It obtains lotion and is heated to 60~90 DEG C, preferably 70~80 DEG C.
Cause the hydrophobic monomer in polymerization High Internal Phase Emulsion, after reaction obtains white solid, uses elution aqueous solvent, second
The mixture of alcohol or water and ethyl alcohol washs solid product, and the porous material with certain pore size can be obtained after drying.
Further, the emulsifier is selected from one of following substance or a variety of: Span80, Span60, polyglycereol alkene
Base succinate or HypermerT96.
Further, the hydrophobic monomer is selected from one of following substance or a variety of: styrene, divinylbenzene,
2-Hydroxyethyl methacrylate, 2-EHA, 2-Ethylhexyl Methacrylate, lauryl acrylate, acrylic acid
Tetradecane base ester, lauryl methacrylate, butyl acrylate, methacrylic acid tetradecane base ester, Glycidyl methacrylate
Glyceride or ethylene glycol dimethacrylate.
Further, the electrolyte is selected from one or both of sodium chloride or calcium chloride.
Further, mass fraction of the emulsifier in oily phase is 5%~30%.
Further, mass fraction of the electrolyte in water phase is 0.5%~3%.
Further, the oil is mutually continuously added into twin-screw respectively and squeezes with the ratio of water phase 1:40~1:3 by volume
Out in machine.
Further, the screw speed of the double screw extruder is 50~350 rpms, and oil is mutually and water phase is in double spiral shells
Temperature in bar extruder is controlled at 20~50 DEG C, and preferably 30~40 DEG C.
The present invention passes through adjusting screw rod revolving speed and barrel temperature, the continuous interior mutually cream of the height for obtaining dispersed phase drop size adjustable
Liquid.Method of the invention is simple and easy, is suitble to continuous production, obtains dispersed phase drop size and its adjustable high interior mutually cream of distribution
Liquid.
By the dispersed phase drop size of optical microscope inspection High Internal Phase Emulsion, using scanning electron microscope (SEM, S-
3400N, JEOL) pattern of bulk polymer porous material is observed, and it is close to utilize digital display solid body densitometer (EDS-300) to measure its
Degree.The quality of bulk polymer open-cell material is measured using the gentle vernier caliper in day respectively and volume and calculates porosity.
The spies such as the dispersed phase drop size of lotion, the aperture of porous material obtained by the method for the present invention, the density of porous material
Property have controllability.
The present invention utilizes good charging performance possessed by double screw extruder, mixing plasticizing capacity, extrusion stability
The features such as, in conjunction with its positive position conveying characteristic to material, double screw extruder is used in lotion for the first time and is continuously prepared, especially
On the lasting emulsifying process of High Internal Phase Emulsion.
Compared with prior art, method of the invention is simple and easy, is suitble to continuous production High Internal Phase Emulsion and its polymer
Porous material, while twin-screw extrusion function provides enough dispersions, distributed rendering, better temperature control, and has good
Good self-cleaning, therefore, the water-in type High Internal Phase Emulsion and polymer porous material quality of the method for the present invention preparation are higher, work
Skill stability is more preferable.
Detailed description of the invention
Fig. 1 is the optical microscope of 1 gained lotion of embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph of 1 gained porous material of embodiment；
Fig. 3 is the optical microscope of 2 gained lotion of embodiment；
Fig. 4 is the scanning electron microscope (SEM) photograph of 2 gained porous material of embodiment；
Fig. 5 is the optical microscope of 3 gained lotion of embodiment；
Fig. 6 is the scanning electron microscope (SEM) photograph of 3 gained porous material of embodiment；
Fig. 7 is the optical microscope of 4 gained lotion of embodiment；
Fig. 8 is the scanning electron microscope (SEM) photograph of 4 gained porous material of embodiment.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
To weigh 100 grams of Spans 80, it is added in the mixture of 1600 grams of styrene and 400 grams of divinylbenzenes, gained has
Machine solution is oily phase.It weighs 300 grams of sodium chloride and 100 grams of potassium peroxydisulfates is added in 8000 grams of distilled water, acquired solution is
Water phase.30 DEG C mutually are separately heated to water phase by oily, then oil is mutually and water phase is according to the feed rate of volume ratio 1:3, passes through perseverance
Stream pump is added in the double screw extruder that cylinder temperature is arranged in 30 DEG C, twin-screw revolving speed is 350 rpms.Water phase is mutually passed through with oil
Cross twin-screw shearing after, at extruder discharging mouth out be High Internal Phase Emulsion.Gained High Internal Phase Emulsion is heated to 70 DEG C,
Cause the monomer in polymerization High Internal Phase Emulsion, reaction obtains white solid, uses elution aqueous solvent, ethyl alcohol or their mixture
Solid product is washed, arrives the porous material with certain pore size after drying.
By the dispersed phase drop size of optical microscope inspection High Internal Phase Emulsion, High Internal Phase Emulsion obtained by the present embodiment
Optical microscope is as shown in Figure 1, as can be seen from FIG. 1, the resulting lotion of the present embodiment divides aqueous phase droplets average diameter to be 48
Micron.
Using the pattern of scanning electron microscope (SEM, S-3400N, JEOL) observation porous material, the present embodiment gained porous material
Scanning electron microscope (SEM) photograph as shown in Fig. 2, can be calculated according to fig. 2, the aperture of resulting porous material is 47 microns.
The quality of gained porous material is measured using the gentle vernier caliper in day respectively and volume and calculates porosity, this reality
The porosity for applying the resulting porous material of example is 77%.
Embodiment 2
To weigh 600 grams of Spans 60,1600 grams of 2-Hydroxyethyl methacrylate and 400 ethylene glycol dimethacrylates are added
In the mixture of ester, gained organic solution is oily phase.It weighs 300 grams of sodium chloride and 300 grams of potassium peroxydisulfates is added to 10000 grams
In distilled water, acquired solution is water phase.30 DEG C mutually are separately heated to water phase by oily, then oil is mutually and water phase is according to volume ratio 1:
4 feed rate is added to the twin-screw that cylinder temperature is arranged in 30 DEG C, twin-screw revolving speed is 100 rpms by constant flow pump and squeezes
Out in machine.Water phase and oil mutually after twin-screw is sheared, at extruder discharging mouth out be High Internal Phase Emulsion.By gained height
Internal phase emulsions are heated to 70 DEG C, cause the monomer in polymerization High Internal Phase Emulsion, and reaction obtains white solid, use elution solvent
Water, ethyl alcohol or their mixture wash solid product, arrive the porous material with certain pore size after drying.
By the dispersed phase drop size of optical microscope inspection High Internal Phase Emulsion, High Internal Phase Emulsion obtained by the present embodiment
Optical microscope is as shown in figure 3, as can be seen from FIG. 3, the resulting lotion of the present embodiment divides aqueous phase droplets average diameter to be 25
Micron.
Using the pattern of scanning electron microscope (SEM, S-3400N, JEOL) observation porous material, the present embodiment gained porous material
Scanning electron microscope (SEM) photograph as shown in figure 4, can be calculated according to Fig. 4, the aperture of resulting porous material is 27 microns.
The quality of gained porous material is measured using the gentle vernier caliper in day respectively and volume and calculates porosity, this reality
The porosity for applying the resulting porous material of example is 82%.
Embodiment 3
To weigh 200 grams of polyglycereol alkenyl succinic acid esters and 100 grams of HypermerT96,1600 grams of acrylic acid 2- second are added
In the mixture of the own ester of base and 400 grams of divinylbenzenes, gained organic solution is oily phase.Weigh 200 grams of sodium chloride and 300 grams of mistakes
Potassium sulfate is added in 10000 grams of distilled water, and acquired solution is water phase.30 DEG C mutually are separately heated to water phase by oily, then
Oily phase and water phase are added to cylinder temperature by constant flow pump and are arranged in 30 DEG C, twin-screw revolving speed according to the feed rate of volume ratio 1:40
For in 150 rpms of double screw extruders.Water phase and oil are mutually after twin-screw is sheared, at extruder discharging mouth out
It is High Internal Phase Emulsion.Gained High Internal Phase Emulsion is heated to 70 DEG C, causes the monomer in polymerization High Internal Phase Emulsion, reaction obtains
White solid washs solid product using elution aqueous solvent, ethyl alcohol or their mixture, certain to having after drying
The porous material in aperture.
By the dispersed phase drop size of optical microscope inspection High Internal Phase Emulsion, High Internal Phase Emulsion obtained by the present embodiment
Optical microscope is as shown in figure 5, as can be seen from FIG. 5, the resulting lotion of the present embodiment divides aqueous phase droplets average diameter to be 74
Micron.
Using the pattern of scanning electron microscope (SEM, S-3400N, JEOL) observation porous material, the present embodiment gained porous material
Scanning electron microscope (SEM) photograph as shown in fig. 6, can be calculated according to Fig. 6, the aperture of resulting porous material is 68 microns.
The quality of gained porous material is measured using the gentle vernier caliper in day respectively and volume and calculates porosity, this reality
The porosity for applying the resulting porous material of example is 96%.
Embodiment 4
To weigh 400 grams of Spans 80,1600 grams of glycidyl methacrylate and 400 grams of dimethacrylate second are added
In the mixture of diol ester, gained organic solution is oily phase.It weighs 50 grams of sodium chloride and 100 grams of potassium peroxydisulfates is added to 10000
Gram distilled water in, acquired solution is water phase.30 DEG C mutually are separately heated to water phase by oily, then oil is mutually and water phase is according to volume
Feed rate than 1:5 is added to the twin-screw that cylinder temperature is arranged in 30 DEG C, twin-screw revolving speed is 50 rpms by constant flow pump
In extruder.Water phase and oil mutually after twin-screw is sheared, at extruder discharging mouth out be High Internal Phase Emulsion.By gained
High Internal Phase Emulsion is heated to 70 DEG C, causes the monomer in polymerization High Internal Phase Emulsion, and reaction obtains white solid, uses elution solvent
Water, ethyl alcohol or their mixture wash solid product, arrive the porous material with certain pore size after drying.
By the dispersed phase drop size of optical microscope inspection High Internal Phase Emulsion, High Internal Phase Emulsion obtained by the present embodiment
Optical microscope is as shown in fig. 7, as can be seen from FIG. 7, the resulting lotion of the present embodiment divides aqueous phase droplets average diameter to be 30
Micron.
Using the pattern of scanning electron microscope (SEM, S-3400N, JEOL) observation porous material, the present embodiment gained porous material
Scanning electron microscope (SEM) photograph as shown in figure 8, can be calculated according to Fig. 8, the aperture of resulting porous material is 32 microns.
The quality of gained porous material is measured using the gentle vernier caliper in day respectively and volume and calculates porosity, this reality
The porosity for applying the resulting porous material of example is 81%.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
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| CN110283580A (en) * | 2019-06-28 | 2019-09-27 | 中国石油大学(华东) | Pour point depression wax-proofing agent and preparation method thereof |
| CN111054317A (en) * | 2019-12-17 | 2020-04-24 | 华东理工大学 | Preparation method of ultra-high porosity polyacrylate porous oil-absorbing material |
| CN111763341A (en) * | 2020-07-06 | 2020-10-13 | 广东海洋大学 | A kind of porous hydrophobic foam material and its preparation method and application |
| CN113943440A (en) * | 2020-07-17 | 2022-01-18 | 台湾创新材料股份有限公司 | Method for fabricating porous microstructures |
| CN114891149A (en) * | 2022-04-12 | 2022-08-12 | 万华化学集团股份有限公司 | Porous structure material for patch type mask base material, patch type mask containing porous structure material and preparation method of patch type mask |
| CN115368875A (en) * | 2022-08-31 | 2022-11-22 | 苏州大学 | A flexible ice-based cold storage composite material and its preparation method |
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| CN113943440B (en) * | 2020-07-17 | 2023-06-23 | 台湾创新材料股份有限公司 | Method for making porous microstructures |
| CN114891149A (en) * | 2022-04-12 | 2022-08-12 | 万华化学集团股份有限公司 | Porous structure material for patch type mask base material, patch type mask containing porous structure material and preparation method of patch type mask |
| CN114891149B (en) * | 2022-04-12 | 2024-02-02 | 万华化学集团股份有限公司 | Porous structure material for patch type mask base material, patch type mask containing porous structure material and preparation method of porous structure material |
| CN115368875A (en) * | 2022-08-31 | 2022-11-22 | 苏州大学 | A flexible ice-based cold storage composite material and its preparation method |
| CN115368875B (en) * | 2022-08-31 | 2023-07-25 | 苏州大学 | Flexible ice-based cold accumulation composite material and preparation method thereof |
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