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A kind of concave polyacrylonitrile nanoparticle and preparation method thereof

A polyacrylonitrile and nanoparticle technology, which is applied in the field of concave polyacrylonitrile nanoparticles and their preparation, can solve the problems of increasing the difficulty of large-scale production and production cost, complicated post-processing process, complicated preparation process, etc., and achieve excellent optical properties. and mechanical properties, simplify the post-processing process, and simplify the synthesis process.

Inactive Publication Date: 2015-11-11
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the hard template method using polymers, inorganic oxides, metal simple substances, etc. Dissolution and other means, which complicate the preparation process, make the effect worse, reduce the efficiency, and increase the difficulty and production cost of large-scale production

Method used

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  • A kind of concave polyacrylonitrile nanoparticle and preparation method thereof
  • A kind of concave polyacrylonitrile nanoparticle and preparation method thereof
  • A kind of concave polyacrylonitrile nanoparticle and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Add 0.8g of hexadecane to 10g of acrylonitrile monomer and mix evenly to form an oil phase. Dissolve 0.1886g of sodium lauryl sulfate in 89.0014g of deionized water to form a water phase.

[0041] (2) Under magnetic stirring at a speed of 1200 rpm, add the oil phase to the water phase at a flow rate of 8 ml / min, and continue stirring for 20 min to form a coarse emulsion.

[0042] (3) Place the coarse emulsion obtained in step (2) in an ice-water bath, use an ultrasonic cell breaker (BRANSONModels450) at a duty cycle of 67% (work for 2 seconds in a duty cycle, stop for 1 second), and output frequency at 20KHz, Under the condition of an output power of 260W, ultrasonic crushing was performed for 6 minutes to obtain acrylonitrile monomer miniemulsion.

[0043] (4) Put the monomer fine emulsion obtained in step (3) into a 250mL four-neck flask, stir, blow nitrogen, add 0.15g of potassium persulfate after heating up to 75°C, and react at constant temperature for 4 hours,...

Embodiment 2

[0047] (1) Add 0.8g of hexadecane to 10g of acrylonitrile monomer and mix evenly to form an oil phase. Dissolve 0.1886g of sodium tetradecyl sulfate in 88.8614g of deionized water to form a water phase.

[0048] (2) Under magnetic stirring at a speed of 800 rpm, add the oil phase to the water phase at a flow rate of 2 ml / min, and continue stirring for 20 min to form a coarse emulsion.

[0049] (3) Place the coarse emulsion obtained in step (2) in an ice-water bath, use an ultrasonic cell breaker (BRANSONModels450) at a duty cycle of 67% (work for 2 seconds in a duty cycle, stop for 1 second), and output frequency at 10KHz, Under the condition of output power of 160W, ultrasonic crushing was carried out for 10 minutes to obtain acrylonitrile monomer miniemulsion.

[0050] (4) Put the monomer fine emulsion obtained in step (3) into a 250mL four-necked flask, stir, blow nitrogen, add 0.01g of potassium persulfate after heating up to 75°C, react at constant temperature for 4 hours...

Embodiment 3

[0054] (1) Add 0.8g of hexadecane to 10g of acrylonitrile monomer and mix evenly to form an oil phase. Dissolve 0.1886g of sodium lauryl sulfate in 88.7114g of deionized water to form a water phase.

[0055] (2) Under magnetic stirring with a rotation speed of about 1500 rpm, add the oil phase to the water phase at a flow rate of 10 ml / min, and continue stirring for 20 min to form a coarse emulsion.

[0056] (3) Place the coarse emulsion obtained in step (2) in an ice-water bath, use an ultrasonic cell breaker (BRANSONModels450) with a working cycle of 67% (working for 2 seconds in a working cycle, stop for 1 second), and an output frequency of 30KHz, Under the condition of output power of 360W, it was ultrasonically crushed for 2 minutes to obtain acrylonitrile monomer miniemulsion.

[0057] (4) Put the monomer fine emulsion obtained in step (3) into a 250mL four-neck flask, stir, blow nitrogen, add 0.3g potassium persulfate after heating up to 75°C, react at constant tempera...

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Abstract

The invention discloses concave polyacrylonitrile nanoparticles and a preparation method thereof. The method comprises the following steps: mixing a polyacrylonitrile monomer with a co-stablizer to form an oil phase; dissolving an emulsifier and a buffer agent in de-ionized water to form a water phase; under the magnetic stirring, adding the oil phase into the water phase at a flow speed of 5-10 ml / min to form a coarse emulsion; finely emulsifying the obtained coarse emulsion by an ultrasonic cell breaking instrument to obtain a polyacrylonitrile monomer fine emulsion; transferring the obtained polyacrylonitrile monomer fine emulsion into a reaction kettle, heating to 50-75 DEG C, adding an initiator, and reacting for 3-8 hours at a constant temperature; washing and performing vacuum drying to obtain the concave polyacrylonitrile nanoparticles. The particle sizes of the concave polyacrylonitrile nanoparticles prepared by the method are about 100-150 nm and the monomer conversion rate is relatively high. According to the method, the concave polyacrylonitrile nanoparticles can be prepared by one-step fine emulsion polymerization reaction only, a synthetic process is simple, the vacuum drying operation is required only in a postprocessing process, and the method is simple and easy to operate.

Description

technical field [0001] The invention relates to a polyacrylonitrile nano particle, in particular to a concave polyacrylonitrile nano particle and a preparation method thereof. Background technique [0002] Polyacrylonitrile has crystallinity and is widely used in the preparation of polyacrylonitrile fiber, commonly known as acrylic fiber. The polyacrylonitrile used for polyacrylonitrile fibers is micron-scale, and nano-scale polyacrylonitrile has been found to have excellent unique properties in the preparation of ultrafiltration membranes, enzyme curing, carbon nanospheres, catalyst supports and pigment encapsulation. focus on. Concave polyacrylonitrile (PAN) nanoparticles are non-spherical hollow nanoparticles, which have the advantages of both hollow particles and nanoparticles, and have the characteristics of higher specific surface area, lower density and excellent optical and mechanical properties. Therefore, it has broad application prospects. [0003] In recent ye...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/44C08F2/26C08J9/28
Inventor 沈慧芳朱爱玉
Owner SOUTH CHINA UNIV OF TECH
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