CN104788710B - A method of the huge capsule of polyacrylonitrile is prepared based on one-step method - Google Patents
A method of the huge capsule of polyacrylonitrile is prepared based on one-step method Download PDFInfo
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- CN104788710B CN104788710B CN201510155877.2A CN201510155877A CN104788710B CN 104788710 B CN104788710 B CN 104788710B CN 201510155877 A CN201510155877 A CN 201510155877A CN 104788710 B CN104788710 B CN 104788710B
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- polyacrylonitrile
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Abstract
The invention discloses a kind of methods for preparing the huge capsule of polyacrylonitrile based on one-step method, include the following steps: polyacrylonitrile being added to N, in dinethylformamide or/and N-Methyl pyrrolidone, it is uniformly mixed, form polyacrylonitrile solution, methyl tricapryl ammonium chloride and silicone oil are added later, is uniformly mixed, forms polyacrylonitrile lotion；Polyacrylonitrile lotion is added in the syringe with dispensing needle head, syringe is placed on peristaltic pump, peristaltic pump foreign minister flow velocity is adjusted and interior phase flow velocity is to stand or rotated to complete solvent displacement and solidification later to enter polyacrylonitrile emulsion droplets in ultrapure water；It is washed again with n-hexane for several times to remove silicone oil, then for several times with ethanol washing, the huge capsule of polyacrylonitrile is obtained after dry.The huge capsule of the polyacrylonitrile being prepared, similar spherical, partial size reaches micron order or more, hollow porous, has high-specific surface area, has broad application prospects in fields such as water process, solvent extraction, biological medicine, energy problems.
Description
Technical field
The present invention relates to polypropylene capsule preparation fields, and in particular to one kind prepares the huge glue of polyacrylonitrile based on one-step method
The method of capsule.
Background technique
Polyacrylonitrile is a kind of important high molecular material presoma, and chemical stability is good, not facile hydrolysis, anti-oxidant, resistance to
Solvent can effectively prevent the infiltration of gas.Porous material, polypropylene are often prepared as matrix using polyacrylonitrile in material science
Nitrile porous material has many advantages, such as resistance to atent solvent, the erosion of resistance to bacterium, excellent thermally and chemically stability.
The method for preparing polyacrylonitrile capsule at present has paddling process, microfluidic method etc..The polyacrylonitrile glue of paddling process preparation
Capsule good dispersion, but size is smaller, sphericity, concentricity and surface flatness are not highly desirable.What microfluidic method obtained
Polyacrylonitrile capsule size is uniform, can preferably control the size of capsule, it can be difficult to obtaining larger size (400um or more)
Capsule, and subsequent process steps are relatively complicated.
Summary of the invention
It is an object of the present invention to provide a kind of methods for preparing the huge capsule of polyacrylonitrile based on one-step method, to solve existing skill
The deficiency of art.
The invention adopts the following technical scheme:
A method of the huge capsule of polyacrylonitrile is prepared based on one-step method, is included the following steps:
Step 1: polyacrylonitrile is added in n,N-Dimethylformamide or/and N-Methyl pyrrolidone, mixing is equal
Even, forming concentration is 0.05gmL-1~0.15gmL-1Polyacrylonitrile solution, later be added methyl tricapryl ammonium chloride and
Silicone oil is uniformly mixed, and forms polyacrylonitrile lotion, wherein methyl tricapryl ammonium chloride additional amount is in 1ml polyacrylonitrile solution
0.08mL~0.12mL, the additional amount of silicone oil are 0.06mL~0.14mL；
Step 2: the polyacrylonitrile lotion of step 1 preparation is added in the syringe with dispensing needle head, by syringe
It is placed on peristaltic pump, adjusting peristaltic pump foreign minister flow velocity is 2mLh-1~10mLh-1, interior phase flow velocity is 0.2uLmin-1~
0.6uL·min-1, polyacrylonitrile emulsion droplets are entered in ultrapure water, are stood later or in 200rpm~500rpm condition backspin
Turn 12h~for 24 hours to complete solvent displacement and solidification；
Step 3: the product that step 2 obtains is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing,
The huge capsule of the polyacrylonitrile is obtained after dry.
The viscosity of silicone oil is 1cst, 5cst or 10cst in step 1.
The internal diameter of the dispensing needle head of syringe is 0.11mm~0.22mm in step 2.
Beneficial effects of the present invention:
1, the present invention is based on the huge capsules of polyacrylonitrile that one-step method is prepared, and similar spherical, partial size reaches micron order
More than, it is hollow porous, there is high-specific surface area, have extensively in fields such as water process, solvent extraction, biological medicine, energy problems
Wealthy application prospect.
2, the method for the present invention step is simple, the time is short, at low cost.The preparation facilities of huge capsule precursor emulsion is simple, easily
In assembly.
3, the method for the present invention controllability is strong, can be by the control of the flow velocity of lotion, concentration and viscosity to the huge of preparation
Partial size, wall thickness of capsule etc. are controlled.
Detailed description of the invention
Fig. 1 is the optical microscope photograph of the huge capsule entirety of polyacrylonitrile prepared by embodiment 1.
Fig. 2 is the optical microscope photograph that the huge capsule of polyacrylonitrile prepared by embodiment 1 is cut.
Fig. 3 is the scanning electron microscope (SEM) photograph of the huge capsule of polyacrylonitrile prepared by embodiment 3.
Specific embodiment
The present invention is done below with reference to embodiment and attached drawing and is further explained.The following example is merely to illustrate this hair
It is bright, but be not used to limit practical range of the invention.
A method of the huge capsule of polyacrylonitrile is prepared based on one-step method, is included the following steps:
Step 1: polyacrylonitrile is added in n,N-Dimethylformamide or/and N-Methyl pyrrolidone, mixing is equal
Even, forming concentration is 0.05gmL-1~0.15gmL-1Polyacrylonitrile solution, later be added methyl tricapryl ammonium chloride and
Silicone oil is uniformly mixed, and forms polyacrylonitrile lotion, wherein methyl tricapryl ammonium chloride additional amount is in 1ml polyacrylonitrile solution
0.08mL~0.12mL, the additional amount of silicone oil are 0.06mL~0.14mL；The viscosity of silicone oil is 1cst, 5cst or 10cst；
Step 2: the polyacrylonitrile lotion of step 1 preparation is added in the syringe with dispensing needle head, by syringe
It is placed on peristaltic pump, adjusting peristaltic pump foreign minister flow velocity is 2mLh-1~10mLh-1, interior phase flow velocity is 0.2uLmin-1~
0.6uL·min-1, polyacrylonitrile emulsion droplets are entered in ultrapure water, are stood later or in 200rpm~500rpm condition backspin
Turn 12h~for 24 hours to complete solvent displacement and solidification；Wherein, the internal diameter of the dispensing needle head of syringe is 0.11mm~0.22mm；
Step 3: the product that step 2 obtains is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing,
The huge capsule of the polyacrylonitrile is obtained after dry.
Embodiment 1
1) polyacrylonitrile 4.5g is weighed, 30ml n,N-Dimethylformamide is added, is uniformly mixed, the surface 3ml is added later
The silicone oil that activating agent methyl tricapryl ammonium chloride and 3ml viscosity are 5cst, is uniformly mixed, and forms polyacrylonitrile lotion；
2) will prepared polyacrylonitrile lotion be added syringe in, on syringe twist a dispensing needle head, syringe needle it is interior
Diameter is 0.11mm；Syringe is placed on peristaltic pump；Adjusting peristaltic pump foreign minister flow velocity is 6mLh-1, interior phase flow velocity is 0.4uL
min-1, emulsion droplets obtained are entered in ultrapure water, are stood overnight to complete solvent displacement and solidification；
3) product of step 2) is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing, it is dry, it obtains
The huge capsule of polyacrylonitrile.
The optical microscope photograph of the huge capsule entirety of polyacrylonitrile manufactured in the present embodiment is as shown in Figure 1, the light cut
It is as shown in Figure 2 to learn microscope photo.The huge capsule of polyacrylonitrile is whole similar spherical, overall diameter average out to 2mm, wall thickness 0.4
~0.8mm, hollow aperture average out to 0.5mm.
Embodiment 2
1) polyacrylonitrile 3.0g is weighed, 30ml N-Methyl pyrrolidone is added, is uniformly mixed, it is living that the surface 3ml is added later
Property agent methyl tricapryl ammonium chloride and 3ml viscosity be 1cst silicone oil, be uniformly mixed, formed polyacrylonitrile lotion；
2) will prepared polyacrylonitrile lotion be added syringe in, on syringe twist a dispensing needle head, syringe needle it is interior
Diameter is 0.11mm；Syringe is placed on peristaltic pump；Adjusting peristaltic pump foreign minister flow velocity is 4mLh-1, interior phase flow velocity is 0.2uL
min-1, emulsion droplets obtained are entered in ultrapure water, are rotated under the conditions of 200rpm overnight to complete solvent displacement and solidification；
3) product of step 2) is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing, it is dry, it obtains
The huge capsule of polyacrylonitrile.
The huge capsule of polyacrylonitrile manufactured in the present embodiment is whole similar spherical, overall diameter average out to 2.16mm, and wall thickness is
0.3~0.7mm, hollow aperture average out to 0.4mm.
Embodiment 3
1) polyacrylonitrile 3.0g is weighed, 15ml N-Methyl pyrrolidone and 15ml n,N-Dimethylformamide is added, is mixed
It closes uniformly, 3ml surfactant methyl tricapryl ammonium chloride and 4ml viscosity is added later as the silicone oil of 5cst, is uniformly mixed, shape
At polyacrylonitrile lotion；
2) will prepared polyacrylonitrile lotion be added syringe in, on syringe twist a dispensing needle head, syringe needle it is interior
Diameter is 0.22mm；Syringe is placed on peristaltic pump；Adjusting peristaltic pump foreign minister flow velocity is 8mLh-1, interior phase flow velocity is 0.6uL
min-1, emulsion droplets obtained are entered in ultrapure water, are rotated under the conditions of 500rpm for 24 hours to complete solvent displacement and solidification；
3) product of step 2) is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing, it is dry, it obtains
The huge capsule of polyacrylonitrile.
The huge capsule of polyacrylonitrile manufactured in the present embodiment is whole similar spherical, overall diameter average out to 2mm, wall thickness 0.5
~0.8mm, hollow aperture average out to 0.5mm；Scanning electron microscope (SEM) photograph is as shown in Figure 3.
Claims (2)
1. a kind of method for preparing the huge capsule of polyacrylonitrile based on one-step method, which comprises the steps of:
Step 1: polyacrylonitrile is added in n,N-Dimethylformamide or/and N-Methyl pyrrolidone, it is uniformly mixed, shape
It is 0.05gmL at concentration-1~0.15gmL-1Polyacrylonitrile solution, methyl tricapryl ammonium chloride and silicone oil are added later,
It is uniformly mixed, forms polyacrylonitrile lotion, wherein methyl tricapryl ammonium chloride additional amount is in 1ml polyacrylonitrile solution
0.08mL~0.12mL, the additional amount of silicone oil are 0.06mL~0.14mL, and the viscosity of silicone oil is 1cst, 5cst or 10cst；
Step 2: being added the polyacrylonitrile lotion of step 1 preparation in the syringe with dispensing needle head, syringe is placed in
On peristaltic pump, adjusting peristaltic pump foreign minister flow velocity is 2mLh-1~10mLh-1, interior phase flow velocity is 0.2uLmin-1~
0.6uL·min-1, polyacrylonitrile emulsion droplets are entered in ultrapure water, are stood later or in 200rpm~500rpm condition backspin
Turn 12h~for 24 hours to complete solvent displacement and solidification；
Step 3: the product that step 2 obtains is washed with n-hexane for several times to remove silicone oil, then for several times with ethanol washing, it is dry
The huge capsule of the polyacrylonitrile is obtained later.
2. the method according to claim 1 for preparing the huge capsule of polyacrylonitrile based on one-step method, which is characterized in that step
The internal diameter of the dispensing needle head of syringe is 0.11mm~0.22mm in two.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1380617A1 (en) * | 2002-07-13 | 2004-01-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Microcomposites and a method for their preparation |
| CN101224403A (en) * | 2007-10-26 | 2008-07-23 | 清华大学 | Method for preparing microcapsule |
| CN102553500A (en) * | 2012-02-06 | 2012-07-11 | 东南大学 | Method for preparing hollow polymer microcapsules based on millifluidics device |
| CN102895924A (en) * | 2012-10-19 | 2013-01-30 | 东南大学 | Preparation method for Chinese parasol spherical empty capsule based on supercutical fluid |
| CN103108902A (en) * | 2010-09-24 | 2013-05-15 | 荷兰联合利华有限公司 | Highly concentrated, spherical biopolymer gel particle suspensions prepared by hipe-gelation process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103736432B (en) * | 2014-01-07 | 2017-01-11 | 东南大学 | Polyacrylonitrile bubble preparation method based on micro-fluidic device |
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2015
- 2015-04-02 CN CN201510155877.2A patent/CN104788710B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1380617A1 (en) * | 2002-07-13 | 2004-01-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Microcomposites and a method for their preparation |
| CN101224403A (en) * | 2007-10-26 | 2008-07-23 | 清华大学 | Method for preparing microcapsule |
| CN103108902A (en) * | 2010-09-24 | 2013-05-15 | 荷兰联合利华有限公司 | Highly concentrated, spherical biopolymer gel particle suspensions prepared by hipe-gelation process |
| CN102553500A (en) * | 2012-02-06 | 2012-07-11 | 东南大学 | Method for preparing hollow polymer microcapsules based on millifluidics device |
| CN102895924A (en) * | 2012-10-19 | 2013-01-30 | 东南大学 | Preparation method for Chinese parasol spherical empty capsule based on supercutical fluid |
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