CN110918977A - Preparation method of nano-gold doped deuterated foam microspheres - Google Patents
Preparation method of nano-gold doped deuterated foam microspheres Download PDFInfo
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- CN110918977A CN110918977A CN201911279007.0A CN201911279007A CN110918977A CN 110918977 A CN110918977 A CN 110918977A CN 201911279007 A CN201911279007 A CN 201911279007A CN 110918977 A CN110918977 A CN 110918977A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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Abstract
The invention discloses a preparation method of a nano-gold doped deuterated foam microsphere, which comprises the following steps: adding deuterated p-divinylbenzene and styrene into a reactor, uniformly mixing, adding an initiator and an organic solvent, stirring, adding gold nanoparticles, a dispersing agent and a water phase, stirring and reacting at 60-120 ℃ for 1-3 hours under the protection of an inert atmosphere, and forming foam pellets in the water phase; and step two, separating the foam beads in the water phase, and then drying to obtain the nano-gold doped deuterated foam microspheres with the foam framework material of deuterated p-divinylbenzene. The nano-gold-doped deuterated foam microsphere provided by the invention has excellent processing formability, the gold element doping distribution is uniform, the specific surface area of the prepared nano-gold-doped deuterated foam microsphere is large, and meanwhile, the preparation method is simple and efficient, and the process difficulty is greatly reduced.
Description
Technical Field
The invention relates to the field of preparation of foam microspheres, in particular to a preparation method of a nano-gold doped deuterated foam microsphere.
Background
The low-density and microporous polymer foam is one of important target materials for Inertial Confinement Fusion (ICF) physical experiments, and has important application in the fields of laser and ion beam physical experiments, laser and substance interaction research, material state equation research and the like. The polymer foam material doped with the heavy metal elements can provide information for physical diagnosis, such as ablation pressure, ablation depth and other important information in the implosion process, and can shield super-thermal electrons. The gold element has stable chemical property and is a metal element with high atomic number required by ICF physical experiment, and high-purity doped polymer foam can be obtained by doping the metal element.
The doping method of the doped polymer foam material mainly comprises physical doping and chemical doping, and the two methods respectively have advantages and disadvantages, for example, although the chemical doping method can prepare foam with uniformly distributed doping elements, the synthesis of the doping element-containing polymerizable monomer is difficult. Other impurity elements are easily introduced by a physical doping method, and the aim of uniformly doping the dopant is difficult to achieve due to agglomeration or sedimentation. Therefore, the search for a simple prepared gold-doped foam material becomes the key of research. At present, the nano-gold-doped foam microspheres have the defects of high processing difficulty, poor foam moldability, low metal doping amount, uneven dispersion and the like.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing nanogold-doped deuterated foam microspheres, comprising the steps of:
adding deuterated p-divinylbenzene and styrene into a reactor, uniformly mixing, adding an initiator and an organic solvent, stirring, adding gold nanoparticles, a dispersing agent and a water phase, stirring and reacting at 60-120 ℃ for 1-3 hours under the protection of an inert atmosphere, and forming foam pellets in the water phase;
and step two, separating the foam beads in the water phase, and then drying to obtain the nano-gold doped deuterated foam microspheres with the foam framework material of deuterated p-divinylbenzene.
Preferably, the mass ratio of the deuterated p-divinylbenzene to the styrene is 2-4: 1; the using amount of the initiator is 1-3% of the mass of the deuterated p-divinylbenzene; the mass-volume ratio of the deuterated p-divinylbenzene to the organic solvent is 1g: 8-15 mL.
Preferably, the mass ratio of the gold nanoparticles to the deuterated p-divinylbenzene is 1: 5-1: 50; the concentration of the dispersing agent in the organic solvent is 2-10 mg/mL; the mass volume ratio of the organic solvent to the water phase is 1: 15-30.
Preferably, the initiator is any one of azobisisobutyronitrile, benzoyl peroxide and azodiisopropyl imidazoline hydrochloride; the organic solvent is any one of dibutyl phthalate, dimethyl phthalate and diethyl phthalate.
Preferably, the particle size of the gold nanoparticles is 10-20 nm; the dispersing agent is any one of poly (4-vinylphenol), oleyl alcohol and n-dodecyl mercaptan; the water phase is a 3-8 wt% polyethylene glycol aqueous solution.
Preferably, in the second step, CO is used for drying2And (5) supercritical drying.
Preferably, in the first step, the gold nanoparticles, the dispersant and the water are mixed and then added into the reactor after the following treatment, wherein the treatment process comprises the following steps: mixing the nano gold particles, the dispersing agent and the water phase, then carrying out high-pressure dispersion treatment, and then carrying out ultrasonic oscillation treatment.
Preferably, the pressure of the high-pressure dispersion treatment is 8000-18000 psi, and the treatment is carried out for 1-3 times; the frequency of the ultrasonic wave is 30-60 KHz, and the power density is 100-500W/cm2The time is 10-30 min.
Preferably, the process in the first step is replaced by: adding deuterated p-divinylbenzene and styrene into a supercritical carbon dioxide reaction device, uniformly mixing, adding an initiator and an organic solvent, stirring, adding gold nanoparticles, a dispersing agent and a water phase, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring and reacting for 30-45 min at the temperature of 60-80 ℃ and the pressure of 20-30 MPa, relieving pressure, and forming foam beads in the water phase.
Preferably, the mass ratio of the deuterated p-divinylbenzene to the styrene is 2-4: 1; the using amount of the initiator is 1-3% of the mass of the deuterated p-divinylbenzene; the mass-volume ratio of the deuterated p-divinylbenzene to the organic solvent is 1g: 3-5 mL; the mass ratio of the gold nanoparticles to the deuterated p-divinylbenzene is 1: 5-1: 50; the concentration of the dispersing agent in the organic solvent is 0.5-1 mg/mL; the volume ratio of the organic solvent to the water phase is 1: 10-12.
The invention at least comprises the following beneficial effects: the nano-gold-doped deuterated foam microsphere provided by the invention has excellent processing formability, the gold element doping distribution is uniform, the specific surface area of the prepared nano-gold-doped deuterated foam microsphere is large, and meanwhile, the preparation method is simple and efficient, and the process difficulty is greatly reduced.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 shows N of nano-gold-doped deuterated foam microspheres prepared in examples 1-4 of the present invention and comparative example 12Schematic diagram of adsorption isotherm curve;
FIG. 2 is a graph showing the trend of the specific surface area of the nano-gold-doped deuterated foam microspheres prepared in examples 1 to 4 and comparative example 1 of the present invention;
FIG. 3 is SEM and EDS images of nano-gold doped deuterated foam microspheres prepared in comparative example 1 of the invention;
FIG. 4 is SEM and EDS diagrams of nano-gold doped deuterated foam microspheres prepared in example 1 of the invention;
FIG. 5 is SEM and EDS images of the nano-Au-doped deuterated foam microsphere prepared in example 5 of the invention;
FIG. 6 is SEM and EDS images of the nano-Au-doped deuterated foam microsphere prepared in example 6 of the invention;
fig. 7 is SEM and EDS images of the au nanoparticle-doped deuterated foam microsphere prepared in example 7 of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding 20mg of 15nm gold nanoparticles, 6mg of dispersant and 60mL of water phase, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam beads in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2Performing supercritical drying to obtain a nano gold doped deuterated foam microsphere with a foam framework material of deuterated p-divinylbenzene; the specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 653.485m2/g。
Example 2:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding 20mg of 15nm gold nanoparticles, 15mg of dispersant and 60mL of water phase, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam beads in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 672.286m2/g。
Example 3:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding 20mg of 15nm gold nanoparticles, 21mg of dispersant and 60mL of water phase, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam beads in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 482.202m2/g。
Example 4:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding 20mg of 15nm gold nanoparticles, 30mg of dispersant and 60mL of water phase, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam beads in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 363.100m2/g。
Comparative example 1:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding 20mg of 15nm gold nanoparticles and 60mL of water phase, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam pellets in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared by the comparative example is 1107.192m2/g。
From the specific surface area data tested in examples 1-4 and comparative example 1, the specific surface area shows a decreasing trend as the addition amount of the dispersant increases; and as can be seen from fig. 3, the gold particles thereof have poor dispersibility and are doped in a small amount; in order to further improve the dispersibility of the gold nanoparticles and further reduce the amount of the dispersing agent on the premise of ensuring the larger specific surface area of the foam microspheres (the smaller the amount of the dispersing agent is, the lower the impurity content of the prepared foam microspheres is), the invention further improves the process specifically in the embodiment 5-7;
example 5:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
the first step,Mixing 20mg of 15nm gold nanoparticles, 6mg of a dispersing agent and 60mL of a water phase, performing high-pressure dispersion treatment, and performing ultrasonic oscillation treatment; the pressure of the high-pressure dispersion treatment is 15000psi, and the treatment is carried out for 2 times; the frequency of the ultrasonic wave is 45KHz, and the power density is 300W/cm2The time is 30 min;
step two, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a reactor, uniformly mixing, adding 6mg of initiator and 3mL of organic solvent, stirring, adding the material treated in the step one, stirring and reacting for 1 hour at 80 ℃ under the protection of inert atmosphere, and forming foam pellets in a water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step three, separating the foam beads in the water phase, and then adopting CO2Performing supercritical drying to obtain a nano gold doped deuterated foam microsphere with a foam framework material of deuterated p-divinylbenzene; the specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 663.857m2(ii)/g, the specific surface area does not change much compared with example 1; however, this example first used a high-pressure dispersion treatment and an ultrasonic oscillation treatment of the gold nanoparticles with a dispersant and an aqueous phase, and as can be seen from a comparison of fig. 4 and 5, the amount of gold nanoparticles doped was made more and more uniform in this manner.
Example 6:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a supercritical carbon dioxide reaction device, uniformly mixing, adding 6mg of initiator and 1.5mL of organic solvent, stirring, adding 20mg of nano-gold particles, 1.5mg of dispersing agent and 18mL of water phase, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring and reacting for 45min at the temperature of 70 ℃ and under the pressure of 25MPa, and decompressing to form foam beads in the water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 685.569m2(ii)/g; by carrying out the reaction in supercritical carbon dioxide, the specific surface area of the prepared nano-gold-doped deuterated foam microsphere is remarkably improved compared with that of example 1 under the condition of relatively less addition of the dispersing agent, and as can be seen from comparison between fig. 4 and fig. 6, the doping amount of the nano-gold particles is more and more uniform in such a way.
Example 7:
a preparation method of a nano-gold doped deuterated foam microsphere comprises the following steps:
step one, mixing 20mg of 15nm gold nanoparticles, 1.5mg of a dispersing agent and 18mL of a water phase, performing high-pressure dispersion treatment, and then performing ultrasonic oscillation treatment; the pressure of the high-pressure dispersion treatment is 15000psi, and the treatment is carried out for 2 times; the frequency of the ultrasonic wave is 45KHz, and the power density is 300W/cm2The time is 30 min;
step one, adding 300mg of deuterated p-divinylbenzene and 100mg of styrene into a supercritical carbon dioxide reaction device, uniformly mixing, adding 6mg of initiator and 1.5mL of organic solvent, stirring, adding the material treated in the step one, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring and reacting for 45min at the temperature of 70 ℃ and under the pressure of 25MPa, and decompressing to form foam pellets in a water phase; the initiator is azobisisobutyronitrile; the organic solvent is dibutyl phthalate; the dispersant is poly (4-vinylphenol); the water phase is a 5 wt% polyethylene glycol aqueous solution;
step two, separating the foam beads in the water phase, and then adopting CO2And (5) performing supercritical drying to obtain the nano-gold doped deuterated foam microsphere with the foam framework material of deuterated p-divinylbenzene. The specific surface area of the nano-gold doped deuterated foam microsphere prepared in the example is 722.168m2(ii)/g; firstly, the nano-gold particles, the dispersant and the water phase are subjected to high-pressure dispersion treatment and ultrasonic oscillation treatment and are reacted in supercritical carbon dioxide, so that the specific surface area of the prepared nano-gold doped deuterated foam microsphere is remarkably improved compared with that of example 1, and as can be seen from comparison between fig. 6 and 7, the doping amount of the nano-gold particles is more and more uniform in such a way.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. A preparation method of a nano-gold doped deuterated foam microsphere is characterized by comprising the following steps:
adding deuterated p-divinylbenzene and styrene into a reactor, uniformly mixing, adding an initiator and an organic solvent, stirring, adding gold nanoparticles, a dispersing agent and a water phase, stirring and reacting at 60-120 ℃ for 1-3 hours under the protection of an inert atmosphere, and forming foam pellets in the water phase;
and step two, separating the foam beads in the water phase, and then drying to obtain the nano-gold doped deuterated foam microspheres with the foam framework material of deuterated p-divinylbenzene.
2. The method for preparing the nanogold-doped deuterated foam microsphere as claimed in claim 1, wherein the mass ratio of deuterated p-divinylbenzene to styrene is 2-4: 1; the using amount of the initiator is 1-3% of the mass of the deuterated p-divinylbenzene; the mass-volume ratio of the deuterated p-divinylbenzene to the organic solvent is 1g: 8-15 mL.
3. The method for preparing the nanogold-doped deuterated foam microsphere as claimed in claim 1, wherein the mass ratio of the nanogold particles to the deuterated p-divinylbenzene is 1:5 to 1: 50; the concentration of the dispersing agent in the organic solvent is 2-10 mg/mL; the volume ratio of the organic solvent to the water phase is 1: 15-30.
4. The method of claim 1, wherein the initiator is any one of azobisisobutyronitrile, benzoyl peroxide, and azodiisopropylimidazoline hydrochloride; the organic solvent is any one of dibutyl phthalate, dimethyl phthalate and diethyl phthalate.
5. The method of claim 1, wherein the gold nanoparticles have a particle size of 10-20 nm; the dispersing agent is any one of poly (4-vinylphenol), oleyl alcohol and n-dodecyl mercaptan; the water phase is a 3-8 wt% polyethylene glycol aqueous solution.
6. The method of claim 1, wherein in the second step, CO is used for drying2And (5) supercritical drying.
7. The method of claim 1, wherein in the first step, the nanogold particles, the dispersant and the water are mixed and added into the reactor after the following treatment, and the treatment process comprises: mixing the nano gold particles, the dispersing agent and the water phase, then carrying out high-pressure dispersion treatment, and then carrying out ultrasonic oscillation treatment.
8. The method for preparing nano-gold-doped deuterated foam microspheres as claimed in claim 1, wherein the pressure of the high-pressure dispersion treatment is 8000-18000 psi for 1-3 times; the frequency of the ultrasonic wave is 30-60 KHz, and the power density is 100-500W/cm2The time is 10-30 min.
9. The method for preparing the nanogold-doped deuterated foam microsphere as recited in claim 1, wherein the process in the first step is replaced by the following steps: adding deuterated p-divinylbenzene and styrene into a supercritical carbon dioxide reaction device, uniformly mixing, adding an initiator and an organic solvent, stirring, adding gold nanoparticles, a dispersing agent and a water phase, injecting carbon dioxide into the supercritical carbon dioxide reaction device, stirring and reacting for 30-45 min at the temperature of 60-80 ℃ and the pressure of 20-30 MPa, relieving pressure, and forming foam beads in the water phase.
10. The method for preparing the nanogold-doped deuterated foam microspheres as claimed in claim 9, wherein the mass ratio of deuterated p-divinylbenzene to styrene is 2-4: 1; the using amount of the initiator is 1-3% of the mass of the deuterated p-divinylbenzene; the mass-volume ratio of the deuterated p-divinylbenzene to the organic solvent is 1g: 3-5 mL; the mass ratio of the gold nanoparticles to the deuterated p-divinylbenzene is 1: 5-1: 50; the concentration of the dispersing agent in the organic solvent is 0.5-1 mg/mL; the volume ratio of the organic solvent to the water phase is 1: 10-12.
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