CN105949397B - The method for forming nanometer abnormal shape particle as matrix using polyaniline - Google Patents
The method for forming nanometer abnormal shape particle as matrix using polyaniline Download PDFInfo
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention discloses the methods for forming nanometer abnormal shape particle as matrix using polyaniline, belong to the fields such as emulsion polymerization and conductive material.The present invention is used using polyaniline as matrix, synthesizes nanometer abnormal shape latex particle by the method for seed mini-emulsion polymerization.Co-stabilizer of the block polymer as mini-emulsion polymerization is used in the preparation process of polyaniline seed miniemulsion, is stabilized aniline drop, so that polyaniline partial size can achieve 30nm or so, is evenly distributed；Use the slow method that mixed monomer solution is added dropwise that can form stable polyaniline as matrix nano latex particle, latex is easy film forming.It is poor to improve polyaniline filming performance, the shortcomings that being unevenly distributed；It uses amphiphilic solvent reflux polyaniline for matrix nano latex particle, increases the phase transfer of inside nanoparticles polyaniline, polyaniline can be migrated in special-shaped particle surface well, improve surface conductivity.
Description
Technical field:
The present invention relates to using polyaniline as matrix, nanometer abnormal shape particle is synthesized by the method for seed mini-emulsion polymerization.This
Kind method is related to the fields such as emulsion polymerization and conductive material.
Background technique:
Electric conductivity is the most important performance of conductive polymer material, and the high molecular synthesis of nano structural conductive is significantly
The electric conductivity of conducting polymer is improved, to widen the application field of conductive polymer material.Nano material combines letter
Breath, the technologies such as biology are fast-developing, play an important role in the multiple fields such as medical treatment and information.On the other hand, by using lotion
Polymerizeing " MOLECULE DESIGN " synthesis has anisotropic approach most important to the development of conductive polymer material.
Anisotropy, also referred to as non-equal tropism refer to the properties such as all or part of physics, the chemistry of object with the difference in direction
And respectively show certain different characteristic.And anisotropic particle, it is particle with the above characteristics.In fact, from
Most granular substance is all anisotropic in right boundary, and exactly this anisotropy imparts the function of their multiplicity
Property.There are many kinds of the preparation methods of anisotropic particles, and the most common preparation method is phase separation method.With it is easy to operate,
The advantages that product range scale is big.The preparation process of phase separation method includes the collective effect of three classes mechanism；Due to the body of polymer
Interaction force caused by product expansion between monomer and condensate；Elastic force interaction between condensate；Particle and continuous
Surface tension between liquid phase.There is be separated from each other, heterogeneity component, or unsymmetric structure inside anisotropic particles；It is internal
Diversity usually realized by nucleocapsid structure, internal coenocytism just can be realized the embedding of heterogeneity component with point
From；Although each structure is spatially mutually indepedent inside particle, it is not superimposed not instead of simply in nature, is remaining different
On the basis of constitutive property essential characteristic, while there is the generated comprehensive performance of synergistic effect between component.This had both been compensated for respectively
The shortcomings that same sex particle, and show new capability not available for isotropism particle.It generally can be poly- using seed emulsion
It closes, emulsifier-free emulsion polymerization, general emulsion polymerization, mini-emulsion polymerization, micro-emulsion polymerization, Pickering emulsion polymerization etc..Thin cream
Liquid polymerization is considered as the most effectual way that particle is coated to polymeric inner.Each drop of miniemulsion may be considered that
It is independent nanometer to micron reaction vessel, the size of drop is generally 50 between 500nm.Therefore, miniemulsion side can be used
Method prepares anisotropy nanometer conductive polymer latex particle, realizes that layer/polyaniline conductive polymer is distributed control in latex particle
It makes, film surface is smooth after film forming, can improve electric conductivity.
Summary of the invention:
The purpose of the present invention is utilization (seed) mini-emulsion polymerization methods to obtain the nanometer anisotropic particles that polyaniline is matrix.
In the method that polyaniline forms nanometer abnormal shape particle as matrix, carry out as steps described below:
(1) preparation of polyaniline seed miniemulsion:
At room temperature, dodecyl benzene sulfonic acid is added in deionized water A, gentle agitation is to being completely dissolved；By block polymerization
Object is dissolved in aniline, is gradually added dropwise in dodecyl benzene sulfonic acid water solution system and is stirred 15min.At room temperature, magnetic force is used
Blender stirs 15min pre-emulsification, and 90% power ultrasound 5min(ice water of 450W ultrasonic cell disrupte machine is cooling), by ammonium persulfate
It is dissolved in deionized water B, and is slowly dropped into system, drip off within 1 hour, system gradually becomes blackish green, is stirred to react 5 hours and ties
Shu Fanying.
Block copolymer is polystyrene and polyacrylate (methyl acrylate, ethyl acrylate, third in step (1)
Olefin(e) acid propyl ester or butyl acrylate) or methacrylate (methyl methacrylate, ethyl methacrylate, methacrylic acid
Propyl ester or butyl methacrylate) based block copolymer, the equal relative molecular weight of polystyrene block polymer number is 500-2000；
The equal relative molecular weight of poly- (methyl) arylate blocks number is 3000-5000.
Wherein the mass ratio of dodecyl benzene sulfonic acid and deionized water A are 2.12:150 in step (1).
Wherein the mass ratio of dodecyl benzene sulfonic acid, block polymer and aniline is 2.12:0.10:0.46 in step (1).
Wherein the mass ratio of dodecyl benzene sulfonic acid, ammonium persulfate and deionized water B is 2.12:1.14 in step (1):
20。
(2) polyaniline is the preparation of matrix nano latex particle:
After the step of polymerization is completed (1) polyaniline seed miniemulsion is nitrogen 30min minutes logical, it is heated with stirring to 70 DEG C；It will
The mixed solution that monomer, crosslinking agent, initiator and solvent form, is slowly added dropwise according to certain speed to the careful cream of polyaniline kind
In liquid, after being added dropwise to complete, reaction solution keeps the temperature 1 hour at 75 DEG C, and reaction was completed.
Monomer in step (2) the method is esters of acrylic acid (methyl acrylate, ethyl acrylate, propyl acrylate
Or butyl acrylate), methyl acrylic ester (methyl methacrylate, ethyl methacrylate, propyl methacrylate or first
Base butyl acrylate) and styrene monomer；Crosslinking agent can be glycol methacrylate, divinylbenzene, trimethyl
Propane trimethyl acrylic ester, pentaerythritol triacrylate, pentaerythritol tetraacrylate and tetraethyl oxosilane etc.；Cause
Agent is azodiisobutyronitrile, azobisisoheptonitrile, cumyl peroxide and benzoyl peroxide etc.；Solvent is toluene, diformazan
The mixed solvent of the one or more such as benzene, ethylbenzene and chloromethanes.
Esters of acrylic acid (methyl acrylic ester) and styrene quality amount ratio are 1.0 in step (2) the method:
2.0-5.0；Dosage of crosslinking agent and styrene quality usage ratio are 0.0005-0.0010:1；Initiator amount and styrene matter
Amount usage ratio is 0.02-0.05:1；Solvent usage and styrene quality usage ratio are 0.10-0.30:1.Mixed solution
Rate of addition be 1.0-2.0 grams/(100 grams of polyaniline seed miniemulsions of hour), time for adding 2 hours.
(3) polyaniline is the formation of matrix abnormal shape nanoparticle:
It is that matrix nano latex is centrifuged 5 minutes using 10000 revs/min of seperators by the polyaniline prepared by step (2), it is real
Existing solid-liquor separation；A certain amount of amphiphilic solvent is added with lower layer's solid, is placed in the reaction kettle equipped with reflux condensing tube, starts
Stirring, stirring rate are 100 r/min., it is heated to amphiphilic solvent reflux temperature, return time 24 hours.After stopping reflux,
Obtaining polyaniline is matrix abnormal shape nanoparticle.
Amphiphilic solvent refer in water in benzene (toluene, ethylbenzene or dimethylbenzene) with certain solubility solvent, such as
Acetone or tetrahydrofuran etc.；Dosage and lower layer's amount of solid quality usage ratio are 10.0-20.0:1.
The advantage of the invention is that the present invention is used using polyaniline as matrix, synthesized by the method for seed mini-emulsion polymerization
The special-shaped latex particle of nanometer.1, use block polymer as mini-emulsion polymerization in the preparation process of polyaniline seed miniemulsion
Co-stabilizer stabilizes aniline drop, so that polyaniline partial size can achieve 30nm or so, is evenly distributed；2, it is added dropwise using slow
It is matrix nano latex particle that the method for mixed monomer solution, which can form stable polyaniline, and latex is easy film forming.It improves
The shortcomings that polyaniline filming performance is poor, is unevenly distributed；3, use amphiphilic solvent reflux polyaniline for matrix nano emulsion particle
Son increases the phase transfer of inside nanoparticles polyaniline, and polyaniline can be migrated in special-shaped particle surface well, improves surface
Conductivity.
Detailed description of the invention
Fig. 1 is 1 polyaniline miniemulsion electronic transmission electron microscopic picture of embodiment；
Fig. 2 is the electronic transmission electron microscopic picture that 1 polyaniline of embodiment is matrix abnormal shape Nano latex；
Fig. 3 is film surface atomic force microscope images after embodiment 1 forms a film.
Specific embodiment
Below with reference to example, the present invention is described in further detail.
Embodiment 1
(1) preparation of polyaniline seed miniemulsion:
At room temperature, 2.12 grams of dodecyl benzene sulfonic acid are added in 150 grams of deionized waters, gentle agitation is to being completely dissolved；
By 0.10 gram of block polymer (polystyrene-methacrylic acid methyl esters block polymer, the equal average molecular of polystyrene block number
Amount is 500；The equal relative molecular weight of poly- (methyl) arylate blocks number is 3000), it is dissolved in 0.46 gram of aniline, is gradually added dropwise
Enter in dodecyl benzene sulfonic acid water solution system and stirs 15min.At room temperature, 15min pre-emulsification is stirred with magnetic stirrer,
90% power ultrasound 5min(ice water of 450W ultrasonic cell disrupte machine is cooling), 1.14 grams of ammonium persulfates are dissolved in 20 grams of deionized waters
In, and be slowly dropped into system, it drips off within 1 hour, system gradually becomes blackish green, and being stirred to react 5 hours, reaction was completed.Fig. 1 is
Polyaniline miniemulsion electronic transmission electron microscopic picture；Black pointing object is polyaniline, and partial size uses Malvern laser diffraction analyzer
The equal average grain diameter of obtained Z is 30 nanometers.
(2) polyaniline is the preparation of matrix nano latex particle:
After the step of polymerization is completed (1) polyaniline seed miniemulsion is nitrogen 30min minutes logical, it is heated with stirring to 70 DEG C；It will
Monomer, crosslinking agent, initiator and solvent composition mixed solution (1.0 grams of methyl acrylate, 2.0 grams of styrene, the double first of ethylene glycol
0.0010 gram of base acrylate, 0.04 gram of azodiisobutyronitrile, 0.2 gram of toluene solvant), according to 1.0 grams/(100 grams of hour poly-
Aniline seed miniemulsion) it is slowly added dropwise into polyaniline seed miniemulsion, time for adding 2 hours, after being added dropwise to complete, reaction solution existed
75 DEG C keep the temperature 1 hour, and reaction was completed.
(3) polyaniline is the formation of matrix abnormal shape nanoparticle:
It is that matrix nano latex is centrifuged 5 minutes using 10000 revs/min of seperators by the polyaniline prepared by step (2), it is real
Existing solid-liquor separation；With 1.0 grams of lower layer's solid, 10.0 grams of acetone are added, is placed in the reaction kettle equipped with reflux condensing tube, is started and stir
It mixes, stirring rate is 100 r/min.57 DEG C of acetone reflux temperature, return time 24 hours of heating.After stopping reflux, gathered
Aniline is matrix abnormal shape nanoparticle.
Fig. 2 is the electronic transmission electron microscopic picture that polyaniline is matrix abnormal shape Nano latex, from the figure, it can be seen that newborn
The equal average grain diameter of the sub- Z of micelle is 240 nanometers.Polyaniline forms special-shaped surfaces.Conductivity is 3.8 × 10-4s/cm.Fig. 3 is implemented
Film surface atomic force microscope images after example 1 forms a film, base altitude is consistent after display forms a film, and film surface is smooth.
Embodiment 2
(1) preparation of polyaniline seed miniemulsion:
At room temperature, 2.12 grams of dodecyl benzene sulfonic acid are added in 150 grams of deionized waters, gentle agitation is to being completely dissolved；
By 0.10 gram of block polymer (polystyrene-methacrylic acid methyl esters block polymer, the equal average molecular of polystyrene block number
Amount is 2000；The equal relative molecular weight of poly- (methyl) arylate blocks number is 5000), it is dissolved in 0.46 gram of aniline, gradually drips
It is added in dodecyl benzene sulfonic acid water solution system and stirs 15min.At room temperature, 15min pre-emulsification is stirred with magnetic stirrer,
90% power ultrasound 5min(ice water of 450W ultrasonic cell disrupte machine is cooling), 1.14 grams of ammonium persulfates are dissolved in 20 grams of deionized waters
In, and be slowly dropped into system, it drips off within 1 hour, system gradually becomes blackish green, and being stirred to react 5 hours, reaction was completed.Partial size is adopted
It is 33 nanometers with the equal partial size of Z that Malvern laser diffraction analyzer obtains.
(2) polyaniline is the preparation of matrix nano latex particle:
After the step of polymerization is completed (1) polyaniline seed miniemulsion is nitrogen 30min minutes logical, it is heated with stirring to 70 DEG C；It will
Monomer, crosslinking agent, initiator and solvent composition mixed solution (1.0 grams of methyl methacrylate, 5.0 grams of styrene, trimethyl
0.0050 gram of propane trimethyl acrylic ester, 0.25 gram of azobisisoheptonitrile, 1.5 grams of ethyl benzene solvent), according to 2.0 grams/(hour
100 grams of polyaniline seed miniemulsions) it is slowly added dropwise into polyaniline seed miniemulsion, time for adding 2 hours, after being added dropwise to complete,
Reaction solution keeps the temperature 1 hour at 75 DEG C, and reaction was completed.
(3) polyaniline is the formation of matrix abnormal shape nanoparticle:
It is that matrix nano latex is centrifuged 5 minutes using 10000 revs/min of seperators by the polyaniline prepared by step (2), it is real
Existing solid-liquor separation；With 1.0 grams of lower layer's solid, 20.0 grams of tetrahydrofuran are added, is placed in the reaction kettle equipped with reflux condensing tube, opens
Dynamic stirring, stirring rate are 100 r/min.It is heated to 66 DEG C of solvent reflux temperature, return time 24 hours.After stopping reflux,
Obtaining polyaniline is matrix abnormal shape nanoparticle.
The equal average grain diameter of particle Z is 260 nanometers.Polyaniline forms special-shaped surfaces.Film surface is smooth after film forming, and conductivity is
3.4×10-4 s/cm。
The above-mentioned description to embodiment is for that can understand and apply the invention convenient for those skilled in the art.
Those skilled in the art obviously easily can make various modifications to these embodiments, and General Principle described herein
It is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to embodiment here, this fields
Technical staff's announcement according to the present invention, the modification made for the present invention all should be within protection scope of the present invention.
Claims (5)
1. the method for forming nanometer abnormal shape particle as matrix using polyaniline, it is characterised in that carry out as steps described below:
(1) preparation of polyaniline seed miniemulsion:
At room temperature, dodecyl benzene sulfonic acid is added in deionized water A, gentle agitation is to being completely dissolved；Block polymer is molten
Solution is gradually added dropwise in dodecyl benzene sulfonic acid water solution system in aniline and stirs 15min；At room temperature, magnetic agitation is used
Machine stirs 15min pre-emulsification, and 90% power ultrasound 5min of 450W ultrasonic cell disrupte machine, ice water is cooling, dissolves ammonium persulfate into
It in ionized water B, and is slowly dropped into system, drips off within 1 hour, system gradually becomes blackish green, and being stirred to react 5 hours terminates instead
It answers；
(2) polyaniline is the preparation of matrix nano latex particle:
After the step of polymerization is completed (1) polyaniline seed miniemulsion is nitrogen 30min minutes logical, it is heated with stirring to 70 DEG C；By monomer,
The mixed solution of crosslinking agent, initiator and solvent composition, is slowly added dropwise according to certain speed into polyaniline seed miniemulsion,
After being added dropwise to complete, reaction solution keeps the temperature 1 hour at 75 DEG C, and reaction was completed；
(3) polyaniline is the formation of matrix abnormal shape nanoparticle:
It is that matrix nano latex is centrifuged 5 minutes using 10000 revs/min of seperators by the polyaniline prepared by step (2), realizes liquid
Gu separation；A certain amount of amphiphilic solvent is added with lower layer's solid, is placed in the reaction kettle equipped with reflux condensing tube, starts and stir
It mixes, stirring rate is 100 r/min；It is heated to amphiphilic solvent reflux temperature, return time 24 hours；After stopping reflux, obtain
It is matrix abnormal shape nanoparticle to polyaniline；
Wherein block copolymer is styrene and (methyl) acrylate based block copolymer in step (1),
Wherein step (2) monomer is styrene and (methyl) acrylic ester monomer.
2. the method according to claim 1 for forming nanometer abnormal shape particle as matrix using polyaniline, it is characterised in that wherein
In step (1) in monomer used in block polymer: esters of acrylic acid is methyl acrylate, ethyl acrylate, propyl acrylate
Or butyl acrylate；Methacrylate is methyl methacrylate, ethyl methacrylate, propyl methacrylate or methyl
Butyl acrylate；The equal relative molecular weight of the number of polystyrene block is 500-2000；Poly- (methyl) arylate blocks number is homogeneous
It is 3000-5000 to molecular weight；
Wherein the mass ratio of dodecyl benzene sulfonic acid and deionized water A are 2.12:150 in step (1)；
Wherein the mass ratio of dodecyl benzene sulfonic acid, block polymer and aniline is 2.12:0.10:0.46 in step (1)；
Wherein the mass ratio of dodecyl benzene sulfonic acid, ammonium persulfate and deionized water B is 2.12:1.14:20 in step (1).
3. the method according to claim 1 for forming nanometer abnormal shape particle as matrix using polyaniline, it is characterised in that wherein
In monomer used in step (2): esters of acrylic acid is methyl acrylate, ethyl acrylate, propyl acrylate or butyl acrylate；
Methyl acrylic ester is methyl methacrylate, ethyl methacrylate, propyl methacrylate or butyl methacrylate；
Crosslinking agent is glycol methacrylate, divinylbenzene, trimethyl propane trimethyl acrylic ester, pentaerythrite 3 third
Olefin(e) acid ester, pentaerythritol tetraacrylate or tetraethyl oxosilane；Initiator is azodiisobutyronitrile, azobisisoheptonitrile, mistake
Aoxidize diisopropylbenzene (DIPB) or benzoyl peroxide；Solvent is one or more of mixed solvents of toluene, dimethylbenzene, ethylbenzene.
4. the method according to claim 1 for forming nanometer abnormal shape particle as matrix using polyaniline, it is characterised in that step
(2) (methyl) esters of acrylic acid and styrene quality amount ratio are 1.0:2.0-5.0 in the method；Dosage of crosslinking agent is benzene second
The 0.0005-0.0010 of alkene quality dosage；Initiator amount is the 0.02-0.05 of styrene quality dosage；Solvent usage is benzene
The 0.10-0.30 of Ethylene mass dosage；The rate of addition of mixed solution be 1.0-2.0 grams/(hour, 100 grams of polyaniline kinds were careful
Lotion), time for adding 2 hours.
5. the method according to claim 1 for forming nanometer abnormal shape particle as matrix using polyaniline, it is characterised in that amphiphilic
Property solvent is acetone or tetrahydrofuran；Dosage is the 10.0-20.0 of lower layer's amount of solid quality dosage.
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| CN101768316A (en) * | 2010-03-04 | 2010-07-07 | 陕西科技大学 | Preparation method of polyaniline/P (MMA-BA-HEA) conductive composite material |
| CN103193991A (en) * | 2013-04-02 | 2013-07-10 | 扬州大学 | Preparation method of bonding polyaniline on surfaces of styrene-acrylate copolymer emulsion particles |
| CN104292374A (en) * | 2013-07-15 | 2015-01-21 | 河北工业大学 | Anisotropic particle preparation method based on change of hydrophilicities of non-crosslinked seeds |
| CN104672368A (en) * | 2015-03-09 | 2015-06-03 | 河北工业大学 | Preparation method of form-adjustable anisotropic asymmetric emulsion particles |
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| US20030215638A1 (en) * | 2001-11-05 | 2003-11-20 | Wm. Marsh Rice University | Reduced symmetry nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101768316A (en) * | 2010-03-04 | 2010-07-07 | 陕西科技大学 | Preparation method of polyaniline/P (MMA-BA-HEA) conductive composite material |
| CN103193991A (en) * | 2013-04-02 | 2013-07-10 | 扬州大学 | Preparation method of bonding polyaniline on surfaces of styrene-acrylate copolymer emulsion particles |
| CN104292374A (en) * | 2013-07-15 | 2015-01-21 | 河北工业大学 | Anisotropic particle preparation method based on change of hydrophilicities of non-crosslinked seeds |
| CN104672368A (en) * | 2015-03-09 | 2015-06-03 | 河北工业大学 | Preparation method of form-adjustable anisotropic asymmetric emulsion particles |
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