CN108047382A - A kind of expanded polystyrene microballoon, fluorescent microsphere and preparation method thereof - Google Patents

A kind of expanded polystyrene microballoon, fluorescent microsphere and preparation method thereof Download PDF

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CN108047382A
CN108047382A CN201810064884.5A CN201810064884A CN108047382A CN 108047382 A CN108047382 A CN 108047382A CN 201810064884 A CN201810064884 A CN 201810064884A CN 108047382 A CN108047382 A CN 108047382A
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solution
mixed liquor
microballoon
swelling
preparation
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CN108047382B (en
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王华林
张涛
张科登
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HUBEI NEW ZONGKE VIRUS DESEASE ENGINEERING TECHNOLOGY Co Ltd
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HUBEI NEW ZONGKE VIRUS DESEASE ENGINEERING TECHNOLOGY Co Ltd
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/12Polymerisation in non-solvents
    • C08F2/16Aqueous medium
    • C08F2/22Emulsion polymerisation
    • C08F2/24Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/26Emulsion polymerisation with the aid of emulsifying agents anionic
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08F257/00Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
    • C08F257/02Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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Abstract

The present invention provides a kind of expanded polystyrene microballoon, fluorescent microsphere and preparation method thereof, and the preparation method of expanded polystyrene microballoon includes:Polystyrene seed microspheres solution ultrasonic disperse is obtained into the first mixed liquor in lauryl sodium sulfate aqueous solution, hexamethylene ultrasonic disperse in lauryl sodium sulfate aqueous solution is obtained into the second mixed liquor, the second mixed liquor is added drop-wise to dropwise in the first mixed liquor and is swollen;Prepared expanded polystyrene microballoon can obtain fluorescent microsphere with quantum dot reaction.Prepared by the method for the present invention expanded polystyrene Microsphere Size is homogeneous, fluorescent microsphere fluorescent effect is good.

Description

A kind of expanded polystyrene microballoon, fluorescent microsphere and preparation method thereof
Technical field
The present invention relates to polystyrene material, more particularly, to a kind of expanded polystyrene microballoon, fluorescent microsphere and its Preparation method.
Background technology
Liquid-phase chip is the new technology that a kind of chip technology is combined with flow cytometry.DNA, antibody etc. are attached to Microsphere surface is combined with determinand as probe, the reporter molecule of fluorescent marker is added, by flow cytometer in the liquid phase Detect microsphere surface fluorescence label.
At present, fluorescent dye is mainly utilized for the coding microball in liquid-phase chip field in the market.It is only being absorbed Higher excitation state could be raised to from ground state after the photon of appropriate energy, light used must be accurate wavelength or color. In addition, fluorescent dye stability is poor, the easily quenching (for example, stronger soda acid or high temperature etc.) under conditions of more badly, And lose fluorescent characteristic.Therefore, the fluorescent microsphere of this kind of liquid-phase chip is using process with certain limitation, and stores Condition is harsh.
And it is used to load the microballoon of the soft material of fluorescence, in preparation process, due to being related to, raw material type is more, process is relatively multiple It is miscellaneous, it is difficult to obtain size uniformity, porosity height and the uniform polystyrene microsphere of hole.
The content of the invention
It is micro- that the present invention provides a kind of expanded polystyrene for overcoming the above problem or solving the above problems at least partly Ball, fluorescent microsphere and preparation method thereof.
The unit of parts by weight in the present invention can be this field conventional weight/mass unit.
According to an aspect of the present invention, a kind of preparation method of expanded polystyrene microballoon is provided, including:
Step S1, polystyrene seed microspheres solution ultrasonic disperse is obtained first in lauryl sodium sulfate aqueous solution Hexamethylene ultrasonic disperse is obtained the second mixed liquor by mixed liquor in lauryl sodium sulfate aqueous solution, by the second mixed liquor by It is added drop-wise in the first mixed liquor and is swollen, to obtain the first swelling solution.
In a preferred embodiment, method of the invention further includes:
Step S2, by dibenzoyl peroxide, dimethyl benzene olefin(e) acid glycol ester, methylbenzene olefin(e) acid, toluene and styrene It is mixed to get the second swelling solution;
Step S3, the second swelling solution is added in the first swelling solution the hybrid reaction system that obtains, to the hybrid reaction body Surfactant and polymerization inhibitor are added in system, is reacted to obtain the final product.
In step sl, seed microspheres solution first is formed by polystyrene seed microballoon is soluble in water, then by seed microballoon Solution is added in lauryl sodium sulfate aqueous solution, and using being ultrasonically treated, so that seed microspheres solution is homogeneously dispersed in In lauryl sodium sulfate aqueous solution, the first mixed liquor is obtained.
In step sl, after seed microballoon and sweller being scattered in lauryl sodium sulfate aqueous solution respectively, then will Second mixed liquor of gained is added drop-wise to dropwise in the first mixed liquor, can effectively improve the homogeneous of seed microspheres swell size Property.
In a preferred embodiment, when preparing the first mixed liquor, the mass percent of seed microspheres solution is 4%- 6%;The mass percent of lauryl sodium sulfate aqueous solution is 0.2%-0.3%.Seed microballoon and lauryl sodium sulfate Mass ratio is (1-3):(1-2).By the seed microspheres solution ultrasonic disperse of debita spissitudo in the dodecyl sulphate of debita spissitudo In sodium water solution, also, seed microballoon and the mass ratio of lauryl sodium sulfate is made to be maintained at suitable scope, make the first mixing The mass concentration of seed microballoon is maintained at suitable scope in liquid, and lauryl sodium sulfate is evenly dispersed in beneficial to seed microballoon In aqueous solution.
In a preferred embodiment, when preparing the second mixed liquor, the quality hundred of lauryl sodium sulfate aqueous solution Divide than being 0.2%-0.3%.Hexamethylene and the mass ratio of lauryl sodium sulfate are (1-3):(1-2).Hexamethylene and dodecane The mass ratio of base sodium sulphate is maintained at suitable scope, can sufficiently be mixed with lauryl sodium sulfate aqueous solution beneficial to hexamethylene It is even, so that when the second mixed liquor is added drop-wise in the first mixed liquor, beneficial to the uniform swelling of seed microballoon.
Hexamethylene is dissolved into sodium dodecyl sulfate solution, and using being ultrasonically treated, so that hexamethylene equably divides It is scattered in lauryl sodium sulfate aqueous solution, obtains the second mixed liquor.Hexamethylene is first dissolved in dodecyl sulphate as sweller It in sodium water solution, then mixes with the first mixed liquor, is conducive to the uniform of seed microballoon and sweller and mixes and seed microballoon Swelling efficiency.
In a preferred embodiment, during supersound process, supersonic frequency can be 80-100w;Supersound process when Between be 5-10min.During polystyrene seed microballoon and hexamethylene are distributed to lauryl sodium sulfate aqueous solution, Using supersound process, the scattered effect of polystyrene seed microballoon or hexamethylene in lauryl sodium sulfate aqueous solution can be improved Fruit.Meanwhile in ultrasonication, the temperature of solution can raise due to ultrasonication, can further be conducive to gather Styrene seed microballoon or hexamethylene are rapidly and uniformly scattered in lauryl sodium sulfate aqueous solution.
In a preferred embodiment, under agitation, the drop the second mixed liquor being added drop-wise in the first mixed liquor Rate of acceleration is 0.5~1mL/min.Drop rate is too fast or excessively slow, can cause the swelling rate of Some seeds microballoon very fast, from And cause the size of the seed microballoon after swelling inhomogenous.
In a preferred embodiment, the mass ratio of polystyrene seed microballoon and hexamethylene is 1:(0.8-1.2).It is poly- The dosage of styrene seed microballoon and hexamethylene is maintained at suitable scope, can effectively regulate and control the size of microballoon.
In a preferred embodiment, the second mixed liquor is added in the first mixed liquor, using mixing magnetic agitation item Under part, 5-8h is swollen;The temperature of swelling is for 25-35 DEG C to get to the first swelling solution.
In step s 2, first take in the styrene that dibenzoyl peroxide is dissolved in, sequentially add dimethacrylate second Diol ester, methacrylic acid and toluene are to get the second swelling solution.
Specifically, toluene acts on, so that seed microballoon forms porous structure as pore-foaming agent with seed microballoon.First Base acrylic acid is acted on polystyrene microsphere, makes polystyrene microsphere carboxylated, carboxyl can be with the amino in biomolecule Group forms stable conjugated biological molecules in a manner of Covalent bonding together, is capable of providing the biology point of preparation solution phase biochip Subcarrier.
In a preferred embodiment, the mass ratio of polystyrene seed microballoon, toluene and styrene is 1:(90~ 110):(90~110).
In a preferred embodiment, the dibenzoyl peroxide of 0.08-0.13 parts by weight is taken to be dissolved in 9-11 parts by weight Styrene in, sequentially add ethylene glycol dimethacrylate, the metering system of 0.4-0.6 parts by weight of 9-11 parts by weight The toluene of acid and 9-11 parts by weight.Make dibenzoyl peroxide, ethylene glycol dimethacrylate, methacrylic acid, toluene and The dosage of styrene is maintained at suitable scope, and dibenzoyl peroxide dosage influences the free radical number generated, and then influences The number of initial reaction stage living chain, living chain, which mutually tangles, generates growth cores, and dosage is excessive, and microspherulite diameter dispersiveness can be caused to become Difference;Ethylene glycol dimethacrylate, methacrylic acid dosage are excessive, and grain size will not increase instead is also present with conjuncted microballoon; Styrene dosage is much, and microspherulite diameter can also increase, but dispersiveness can be deteriorated;Toluene dosage is excessive, can become microballoon aperture Greatly or even microsphere breakage can be made.Wherein, methacrylic acid is function monomer, and the dosage of dosage and polystyrene microsphere is kept In rational scope, it can avoid occurring the phenomenon that being separated, microsphere surface collapses in polymerization process.
In a preferred embodiment, the dibenzoyl peroxide of 0.09-0.11 parts by weight is taken to be dissolved in 9-11 parts by weight Styrene in, sequentially add ethylene glycol dimethacrylate, the metering system of 0.4-0.6 parts by weight of 9-11 parts by weight The toluene of acid and 9-11 parts by weight.
In a preferred embodiment, in step S3, after the second swelling solution is added in the first swelling solution, gained mixing Liquid is scattered in the lauryl sodium sulfate aqueous solution that 80mL mass percents are 0.2%-0.3%, and under the conditions of 25-35 DEG C Swelling 8-12h obtains hybrid reaction system.
In a preferred embodiment, surfactant and polymerization inhibitor are added into hybrid reaction system, it can be into one The size of hole in expanded polystyrene microballoon and microballoon prepared by step control.
In a preferred embodiment, polyvinylpyrrolidone can be used in surfactant.
In a preferred embodiment, methylene blue aqueous solution can be used in polymerization inhibitor.
In a preferred embodiment, the quality of polystyrene seed microballoon, polyvinylpyrrolidone and methylene blue Than for 1:(18~22):(0.02~0.05).Specifically, the dosage of surfactant and polymerization inhibitor, it is micro- with polystyrene seed The amount of ball is maintained at corresponding ratio, microspherulite diameter can be made more homogeneous, dispersiveness is more to avoid more polymer chains are generated It is good.
In a preferred embodiment, polyvinylpyrrolidone, the 380-420mL matter of 1.5-2.3 parts by weight are taken successively Amount percentage is that the methylene blue aqueous solution of 0.3%-1.2% and 50-100mL ultra-pure waters are added in glass container, fully After mixing, it is added in hybrid reaction system, under the conditions of 70-100 DEG C, polymerisation 10-15h can obtain porous polyphenyl second Alkene microballoon.
In a preferred embodiment, use 500-800mL ethyl alcohol in supersonic frequency for 80- reaction products therefrom Ultrasound 10-20min is disperseed under the conditions of 100w;Then, it is the ethanol solution of 70%-98% to above-mentioned to use percent by volume Molten product carries out 3-5 centrifuge washing, centrifugal condition 6000-8000r/min, centrifugation time 15-30min;Afterwards, using body The ethanol solution that product percentage is 5%-30% screens above-mentioned product gravity 3-5 times to get few to impurity, size uniformity it is more Hole polystyrene microballoon.
In a preferred embodiment, a kind of preparation method of expanded polystyrene microballoon, including:
Step S1, polystyrene seed microspheres solution ultrasonic disperse is obtained first to mix in sodium dodecyl sulfate solution Close liquid, hexamethylene ultrasonic disperse obtained into the second mixed liquor in sodium dodecyl sulfate solution, by the second mixed liquor 0.5~ The speed of 1mL/min is added drop-wise to dropwise in the first mixed liquor, and magnetic agitation, swelling 5-8h obtain the first swelling solution;
Step S2, it is 1 by mass ratio:(90~110):(3~5):(90~110):The diphenyl peroxide first of (90~110) Acyl, dimethyl benzene olefin(e) acid glycol ester, methylbenzene olefin(e) acid, toluene and styrene are mixed to get the second swelling solution;
Step S3, the second swelling solution is added in the first swelling solution, gained mixed liquor is scattered in lauryl sodium sulfate It in aqueous solution, and is swollen 8-12h under the conditions of 25-35 DEG C and obtains hybrid reaction system, added in into the hybrid reaction system Surfactant and polymerization inhibitor are warming up to 70-100 DEG C of polymerisation 10-15h to obtain the final product.
The present invention also provides a kind of expanded polystyrene microballoons, are prepared by above-mentioned preparation method.The porous polyphenyl The size of ethylene microballoon is 7~8 μm.
The present invention also provides a kind of fluorescent microsphere, which includes above-mentioned expanded polystyrene microballoon and is coated on Quantum dot in the hole of the expanded polystyrene microballoon.The species of quantum dot can be commercially available quantum dot, can be according to reality Border demand is adjusted.
In a preferred embodiment, the content of quantum dot is 50-60% in fluorescent microsphere.
The present invention also provides a kind of preparation method of fluorescent microsphere, by above-mentioned expanded polystyrene microballoon be scattered in chloroform with In the mixed solution of isopropanol, and add in quantum dot solution to obtain the final product.Wherein, in mixed solution, the volume ratio of chloroform is 90- 95%.When preparing fluorescent microsphere, acted on using the preparation-obtained expanded polystyrene microballoon of the present invention with quantum dot, quantum dot It can be good at being fused in the hole of polystyrene microsphere, so as to enhance the fluorescent effect of fluorescent microsphere.
Beneficial effects of the present invention are mainly as follows:
Expanded polystyrene microballoon of the present invention and preparation method thereof, can be prepared size uniformity, hole and hole The expanded polystyrene microballoon of size uniform, preparation process is easily controllable, and the fluorescent effect of obtained fluorescent microsphere is good.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for the expanded polystyrene microballoon being prepared according to the embodiment of the present invention 1;
Fig. 2 is the fluorescence intensity figure for the fluorescent microsphere being prepared according to the embodiment of the present invention 4;
Fig. 3 is the scanning electron microscope (SEM) photograph for the expanded polystyrene microballoon being prepared according to comparative example 1 of the present invention.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is described in further detail.Following embodiment is used for Illustrate the present invention, but be not limited to the scope of the present invention.
Embodiment 1
The present embodiment provides a kind of expanded polystyrene microballoon and preparation method thereof, this method includes following three steps:
(1) the polystyrene seed microspheres solution 2mL ultrasonic disperses that mass percent is 5% are taken in 20mL mass percents The first mixed liquor is obtained for 0.25% lauryl sodium sulfate aqueous solution;128 μ L hexamethylene ultrasonic emulsifications is taken to be scattered in 20mL matter Amount percentage obtains the second mixed liquor for 0.25% lauryl sodium sulfate aqueous solution, by the second mixed liquor with the speed of 0.8mL/min Degree is added dropwise in the first mixed liquor, and magnetic agitation, swelling 6h obtain the first swelling solution under the conditions of 30 DEG C;
(2) 0.1g dibenzoyl peroxides is taken to be dissolved in 10g styrene, sequentially add 10g ethylene glycol dimethacrylate, 0.5g methacrylic acids, 10g toluene, obtain the second swelling solution after mixing;
(3) the second swelling solution is added in the first swelling solution, 80mL mass percents are redispersed in after mixing is In 0.25% lauryl sodium sulfate aqueous solution, and continue under the conditions of 30 DEG C to be swollen the hybrid reaction system of 10h;2g is gathered After vinylpyrrolidone, the methylene blue aqueous solution that 400 μ L mass percents are 0.5% and the mixing of 80mL ultra-pure waters, it is added to In hybrid reaction system, 80 DEG C are warming up to, polymerisation 12h.
500-800mL ethyl alcohol ultrasound 15min under the conditions of supersonic frequency is 90w is used to be divided reaction products therefrom It dissipates;Then, percent by volume is used to carry out 5 centrifuge washings to above-mentioned product for 95% ethanol solution, centrifugal condition is 7000r/min, centrifugation time 25min;Afterwards, percent by volume is used to be screened for 10% ethanol solution to above-mentioned product gravity 5 times to get, the expanded polystyrene microballoon of size uniformity few to impurity.The scanning electron microscope (SEM) photograph of gained expanded polystyrene microballoon See Fig. 1.As seen from Figure 1, the size uniformity of thus obtained microsphere, distribution of pores and pore-size are uniform.
Embodiment 2
The present embodiment provides a kind of expanded polystyrene microballoon and preparation method thereof, this method includes following three steps:
(1) the polystyrene seed microspheres solution 2mL ultrasonic disperses that mass percent is 5% are taken in 20mL mass percents The first mixed liquor is obtained for 0.25% lauryl sodium sulfate aqueous solution;140 μ L hexamethylene ultrasonic emulsifications is taken to be scattered in 20mL matter Amount percentage obtains the second mixed liquor for 0.25% lauryl sodium sulfate aqueous solution, by the second mixed liquor with the speed of 0.6mL/min Degree is added dropwise in the first mixed liquor, and magnetic agitation, swelling 6h obtain the first swelling solution under the conditions of 30 DEG C;
(2) 0.12g dibenzoyl peroxides is taken to be dissolved in 11g styrene, sequentially add 9g ethylene glycol dimethacrylate, 0.4g methacrylic acids, 11g toluene, obtain the second swelling solution after mixing;
(3) the second swelling solution is added in the first swelling solution, 80mL mass percents are redispersed in after mixing is In 0.25% lauryl sodium sulfate aqueous solution, and continue under the conditions of 30 DEG C to be swollen the hybrid reaction system of 11h;2g is gathered After vinylpyrrolidone, the methylene blue aqueous solution that 400 μ L mass percents are 0.75% and the mixing of 80mL ultra-pure waters, it is added to In hybrid reaction system, 80 DEG C are warming up to, polymerisation 12h.
500-800mL ethyl alcohol ultrasound 15min under the conditions of supersonic frequency is 90w is used to be divided reaction products therefrom It dissipates;Then, percent by volume is used to carry out 5 centrifuge washings to above-mentioned product for 95% ethanol solution, centrifugal condition is 7000r/min, centrifugation time 25min;Afterwards, percent by volume is used to be screened for 10% ethanol solution to above-mentioned product gravity 5 times to get, the expanded polystyrene microballoon of size uniformity few to impurity.
Embodiment 3
The present embodiment provides a kind of expanded polystyrene microballoon and preparation method thereof, this method includes following three steps:
(1) the polystyrene seed microspheres solution 2.4mL ultrasonic disperses that mass percent is 5% are taken in 20mL mass percentages Than obtaining the first mixed liquor for 0.25% lauryl sodium sulfate aqueous solution;128 μ L hexamethylene ultrasonic emulsifications is taken to be scattered in 20mL Mass percent obtains the second mixed liquor for 0.25% lauryl sodium sulfate aqueous solution, by the second mixed liquor with 0.8mL/min's Speed is added dropwise in the first mixed liquor, and magnetic agitation, swelling 6h obtain the first swelling solution under the conditions of 30 DEG C;
(2) 0.11g dibenzoyl peroxides is taken to be dissolved in 9g styrene, sequentially add 10g ethylene glycol dimethacrylate, 0.4g methacrylic acids, 11g toluene, obtain the second swelling solution after mixing;
(3) the second swelling solution is added in the first swelling solution, 80mL mass percents are redispersed in after mixing is In 0.25% lauryl sodium sulfate aqueous solution, and continue under the conditions of 30 DEG C to be swollen the hybrid reaction system of 11h;By 2.2g After polyvinylpyrrolidone, the methylene blue aqueous solution that 400 μ L mass percents are 1% and the mixing of 80mL ultra-pure waters, it is added to In hybrid reaction system, 80 DEG C are warming up to, polymerisation 12h.
500-800mL ethyl alcohol ultrasound 15min under the conditions of supersonic frequency is 90w is used to be divided reaction products therefrom It dissipates;Then, percent by volume is used to carry out 5 centrifuge washings to above-mentioned product for 95% ethanol solution, centrifugal condition is 7000r/min, centrifugation time 25min;Afterwards, percent by volume is used to be screened for 10% ethanol solution to above-mentioned product gravity 5 times to get, the expanded polystyrene microballoon of size uniformity few to impurity.
Embodiment 4
This example provides a kind of fluorescent microsphere and preparation method thereof, which is specially:It will be prepared into embodiment 1 To expanded polystyrene microballoon be scattered in the mixed solution of chloroform and isopropanol, and add in quantum dot solution to obtain the final product;Wherein, The volume ratio of chloroform is 95% in mixed solution.The content of quantum dot is 55% in preparation-obtained fluorescent microsphere, fluorescence Intensity map is shown in Fig. 2.
Comparative example 1
This comparative example provides a kind of expanded polystyrene microballoon and preparation method thereof, uses side same as Example 1 Method prepares expanded polystyrene microballoon, the difference is that only:Second mixed liquor is directly disposably poured into the first mixed liquor In.The scanning electron microscope (SEM) photograph of gained expanded polystyrene microballoon is shown in Fig. 3.
Finally, method of the invention is only preferable embodiment, is not intended to limit the scope of the present invention.It is all Within the spirit and principles in the present invention, any modifications, equivalent replacements and improvements are made should be included in the protection of the present invention Within the scope of.

Claims (10)

1. a kind of preparation method of expanded polystyrene microballoon, which is characterized in that including:
Polystyrene seed microspheres solution ultrasonic disperse is obtained into the first mixed liquor in lauryl sodium sulfate aqueous solution, by ring Hexane ultrasonic disperse obtains the second mixed liquor in lauryl sodium sulfate aqueous solution, and the second mixed liquor is added drop-wise to first dropwise It is swollen in mixed liquor.
2. preparation method as described in claim 1, which is characterized in that the rate being added dropwise dropwise is 0.5~1mL/min.
3. preparation method as claimed in claim 2, which is characterized in that the mass ratio of polystyrene seed microballoon and hexamethylene is 1:(0.8-1.2)。
4. such as claim 1-3 any one of them preparation methods, which is characterized in that the second mixed liquor is added drop-wise to first dropwise Swelling obtains the first swelling solution in mixed liquor, and the second swelling solution, the second swelling solution bag are added into first swelling solution Include toluene and styrene;The mass ratio of polystyrene seed microballoon, toluene and styrene is 1:(90~110):(90~110).
5. preparation method as claimed in claim 4, which is characterized in that the second swelling solution is mixed to get with the first swelling solution and mixes Mixed liquor is scattered in lauryl sodium sulfate aqueous solution by liquid, and 8~12h is swollen at 25~35 DEG C and obtains hybrid reaction system.
6. such as claim 1-5 any one of them preparation methods, which is characterized in that add table into the hybrid reaction system Face activating agent and polymerization inhibitor;
Surfactant be polyvinylpyrrolidone and/or, polymerization inhibitor be methylene blue aqueous solution;
The mass ratio of polystyrene seed microballoon, surfactant and polymerization inhibitor is 1:(18~22):(0.02~0.05).
7. preparation method as described in claim 1, which is characterized in that including:
Step S1, polystyrene seed microspheres solution ultrasonic disperse is obtained into the first mixing in sodium dodecyl sulfate solution Hexamethylene ultrasonic disperse is obtained the second mixed liquor by liquid in sodium dodecyl sulfate solution, by the second mixed liquor with 0.5~ The speed of 1mL/min is added drop-wise to dropwise in the first mixed liquor, and magnetic agitation, swelling 5-8h obtain the first swelling solution;
Step S2, it is 1 by mass ratio:(90~110):(3~5):(90~110):The dibenzoyl peroxide of (90~110), Dimethyl benzene olefin(e) acid glycol ester, methylbenzene olefin(e) acid, toluene and styrene are mixed to get the second swelling solution;
Step S3, the second swelling solution is added in the first swelling solution, it is water-soluble that gained mixed liquor is scattered in lauryl sodium sulfate 8-12h being swollen under the conditions of 25-35 DEG C in liquid and obtaining hybrid reaction system, surface-active is added in into the hybrid reaction system Agent and polymerization inhibitor are warming up to 70-100 DEG C of polymerisation 10-15h to obtain the final product.
8. the expanded polystyrene microballoon that any one of the claim 1-7 preparation methods are prepared, the porous polyphenyl second The size of alkene microballoon is 7~8 μm.
9. a kind of fluorescent microsphere, which is characterized in that including expanded polystyrene microballoon as claimed in claim 8 and be coated on Intrapore quantum dot in the expanded polystyrene microballoon;
The content of quantum dot is 50-60% in the fluorescent microsphere.
10. the preparation method of fluorescent microsphere as claimed in claim 9, which is characterized in that be scattered in expanded polystyrene microballoon In the mixed solution of chloroform and isopropanol, and add in quantum dot solution to obtain the final product;
Wherein, in the mixed solution, the volume ratio of chloroform is 90-95%.
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CN113278194A (en) * 2021-05-17 2021-08-20 苏州英芮诚生化科技有限公司 Preparation method of monodisperse magnetic polystyrene microsphere, microsphere and application thereof

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