CN108084314B - P (AAEM-St) coated heart-shaped nano palladium particle composite material - Google Patents
P (AAEM-St) coated heart-shaped nano palladium particle composite material Download PDFInfo
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- CN108084314B CN108084314B CN201710264443.5A CN201710264443A CN108084314B CN 108084314 B CN108084314 B CN 108084314B CN 201710264443 A CN201710264443 A CN 201710264443A CN 108084314 B CN108084314 B CN 108084314B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/282—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing two or more oxygen atoms
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Abstract
The invention discloses a preparation method of a P (AAEM-St) coated heart-shaped nano palladium particle composite material, which comprises weighing PdCl2Dissolving with deionized water, adding AAEM and styrene, adding deionized water, stirring uniformly, adding an initiator, performing ultrasonic treatment, slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample. The P (AAEM-St) coated heart-shaped nano palladium particle composite material is prepared under the conditions that no reducing agent, emulsifier or nitrogen protection is added. Interaction force exists between two carbonyl oxygen atoms and palladium atoms in the long chain of the substrate P (AAEM-St), and palladium atoms are induced to agglomerate to form heart-shaped nano palladium particles. Due to the existence of the defect structure of the central nano palladium particles of the composite material, the nano palladium particles have better thermal catalytic performance, and the thermal degradation of a substrate P (AAEM-St) is promoted.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of a P (AAEM-St) coated heart-shaped nano palladium particle composite material.
Background
The nano metal/polymer composite material is formed by dispersing nano metal particles in a polymer matrix, has the excellent characteristics of the nano metal particles and the polymer, can generate special effects on the physical and chemical properties of the material by regulating and controlling the variable structure parameters of the polymer and the nano particles and utilizing the composite effect of the polymer and the nano particles, thereby endowing the material with unique thermal property, electrical property, optical property, mechanical property, magnetic property, superconducting property and the like, and can be widely applied to the fields of photonics, electronics, enviroment, biomedicine, information materials science and the like.
The nano palladium attracts attention as a good hydrogen storage material and a good conductive slurry, especially as a heterogeneous catalytic material, and the technology for preparing the nano palladium is more and more important along with the application of the nano palladium in the field of heterogeneous catalysis.
Acetoacetoxy Ethyl Methacrylate (AAEM) is a special polymer precursor, is a strong chelating agent, contains high-activity methacrylate groups, has a homopolymer with good thermal stability, and can effectively protect stabilized inorganic nanoparticles by using PAAEM as a matrix. The search shows that the ZrO with the core-shell structure is successfully prepared by using AAEM and styrene copolymer as the stabilizer2PAAEM/PS nanoparticles.
The polymer-coated nano palladium particle composite material is prepared in a palladium salt reaction solution in the presence of various media by ultrasonic, and nano metal palladium particles are prepared by adopting an ultrasonic technology, so that the nano metal palladium particles have smaller particle size and narrower particle size distribution than nano particles prepared by other methods, but some of the methods use reducing agents such as myristyl trimethylamine bromide, ascorbic acid and the like, not only participate in chemical reaction, but also cause the acceleration of ion reduction, the formed seed crystal is larger, the formed crystal is difficult to diffuse, the agglomeration phenomenon occurs, and the particle size of the nano palladium is increased; the researchers prepared the nano palladium particles under the protection of a certain inert atmosphere, but the preparation system becomes complicated. The prepared polymer-coated nano palladium particles are all cylindrical, spherical or nearly spherical in the current literature report.
Disclosure of Invention
Based on the technical problems in the prior art, the invention aims to provide a P (AAEM-St) coated heart-shaped nano palladium particle composite material, wherein a P (AAEM-St) polymer induces nano palladium particles to form a heart-shaped structure.
The second purpose of the invention is to provide a preparation method of the P (AAEM-St) coated heart-shaped nano palladium particle composite material.
A preparation method of a P (AAEM-St) coated heart-shaped nano palladium particle composite material comprises the following steps:
1) AAEM pretreatment: putting the AAEM into a separating funnel, washing the AAEM3-4 times by using deionized water, removing a polymerization inhibitor in the AAEM, and putting a lower layer liquid into a clean conical flask for later use;
2) weighing PdCl2Adding deionized water for dissolving, then adding AAEM and styrene, adding deionized water for the second time, stirring uniformly, and then adding an initiator;
3) ultrasonic treatment: obtaining a reaction solution;
4) washing and drying: slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample.
Preferably, the PdCl in step 2)2The addition proportions of the primary deionized water, the AAEM, the styrene, the secondary deionized water and the initiator are as follows: 0.020-0.080g, 15-25mL, 0.8-1.2mL, 2-8mL, 25-35mL, and 0.008-0.015 g.
Preferably, the PdCl in step 2)2The addition ratio of the primary deionized water, the AAEM, the styrene, the secondary deionized water and the initiator is 0.050g, 20mL, 1mL, 5mL, 30mL and 0.012 g.
Preferably, the initiator in step 2) is potassium persulfate or azobisisobutyronitrile.
Preferably, the step 3) sonication conditions are: working time is 40-60min, ultrasonic treatment is 1s, intermittence is 1s, power is 36%, and temperature is 40-45 ℃.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the P (AAEM-St) -coated heart-shaped nano palladium particle composite material is prepared without adding any reducing agent and emulsifier or using nitrogen for protection, and interaction force exists between two carbonyl oxygen atoms and palladium atoms in a long chain of a substrate P (AAEM-St) to induce palladium atoms to agglomerate to form heart-shaped nano palladium particles. Due to the existence of the defect structure of the central nano palladium particles of the composite material, the nano palladium particles have better thermal catalytic performance, and the thermal degradation of a substrate P (AAEM-St) is promoted.
Drawings
FIG. 1 is a TEM picture of P (AAEM-St) coated heart-shaped nano-palladium particle composite material in example 3;
FIG. 2 is an XPS spectrum of Pd3d in the P (AAEM-St) coated cardioid nano-palladium particle composite of example 3;
FIG. 3 is an XPS fit spectrum of O1s in the P (AAEM-St) coated cardioid nano-palladium particle composite of example 3;
FIG. 4 is a TG curve of P (AAEM-St) (a) and P (AAEM-St) coated cardioid nano-palladium particle composite (b) in example 3;
FIG. 5 is the XRD spectrum of P (AAEM-St) coated heart-shaped nano palladium particle composite material in example 3.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
1. The raw material sources are as follows: PdCl2Analytically pure, Shanghai Yinyuan chemical Co., Ltd; AAEM, 95% alatin; styrene, chemically pure, west longa chemical ltd; azobisisobutyronitrile, analytically pure, jonan shouda chemical ltd; potassium persulfate, analytically pure, bodi chemical ltd, Tianjin; absolute ethanol, analytically pure, stannless, asian chemical limited company.
2. The instrument equipment comprises: JA2003N electronic balance, shanghai precision scientific instruments ltd; XD-1800D ultrasonic cell disruptor, manufactured by Nanjing Europe instruments Ltd.
Example 1
1) AAEM pretreatment: weighing 10mLAAEM, placing the weighed 10mLAAEM into a 60mL separating funnel, washing AAEM for 3 times by using deionized water, removing a polymerization inhibitor in the AAEM, and placing lower-layer liquid into a clean conical bottle for later use;
2) weighing 0.020g of PdCl2Adding 15mL of deionized water for dissolution at one time, then adding 0.8mL of LAAEM and 2mL of styrene, adding 25mL of deionized water at the second time, stirring uniformly, and then adding 0.008g of potassium persulfate;
3) ultrasonic treatment: the treatment conditions are a mode phi 22, the working time is 40min, the ultrasound is 1s, the intermission is 1s, the power is 36 percent, and the temperature is 40 ℃, so that reaction liquid is obtained;
4) washing and drying: slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample.
Example 2
1) AAEM pretreatment: weighing 10mLAAEM, placing the weighed 10mLAAEM into a 60mL separating funnel, washing AAEM for 4 times by using deionized water, removing a polymerization inhibitor in the AAEM, and placing lower-layer liquid into a clean conical bottle for later use;
2) weighing 0.080gPdCl2Adding 25mL of deionized water for dissolving, then adding 1.2mL of LAAEM and 8mL of styrene, adding 35mL of deionized water for the second time, stirring uniformly, and then adding 0.015g of azobisisobutyronitrile;
3) ultrasonic treatment: the treatment conditions are a mode phi 22, the working time is 50min, the ultrasound is 1s, the intermission is 1s, the power is 36 percent, and the temperature is 43 ℃, so that reaction liquid is obtained;
4) washing and drying: slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample.
Example 3
1) AAEM pretreatment: weighing 10mLAAEM, placing the weighed 10mLAAEM into a 60mL separating funnel, washing AAEM for 3 times by using deionized water, removing a polymerization inhibitor in the AAEM, and placing lower-layer liquid into a clean conical bottle for later use;
2) weigh 0.050gPdCl2Adding 20mL of deionized water for dissolution at one time, then adding 1.0mL of LAAEM and 5mL of styrene, adding 30mL of deionized water at the second time, stirring uniformly, and then adding 0.012g of potassium persulfate;
3) ultrasonic treatment: the treatment conditions are a mode phi 22, the working time is 60min, the ultrasound is 1s, the intermission is 1s, the power is 36 percent, and the temperature is 45 ℃ to obtain reaction liquid;
4) washing and drying: slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample.
Preparation of P (AAEM-St) composite material
To 50mL of deionized water, 1mL of AAEM and 5mL of styrene were added, followed by stirring to uniformity, and 0.012g of potassium persulfate was added. The ultrasonic treatment conditions are a mode phi 22, the working time is 60min, the ultrasonic treatment is carried out for 1s, the intermission is 1s, the power is 36 percent, and the temperature is 45 ℃ to obtain reaction liquid; slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for multiple times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading into a sample.
Performance analysis of P (AAEM-St) coated heart-shaped nano palladium particle composite material
Referring to fig. 1, the dark color is nano-palladium, the light color is P (AAEM-St), and P (AAEM-St) is arranged around the heart-shaped nano-Pd, and the irregular light and dark stripes are that the heart-shaped nano-palladium reacts on the polymer, so that the polymer is selectively distributed on the surface, which indicates that the heart-shaped nano-palladium interacts with the substrate P (AAEM-St).
Referring to fig. 2, fig. 2 is an energy spectrum of Pd3d, which is increased by 0.99eV from the peak position (337.5eV) of standard Pd3d and moves toward high energy binding energy, indicating that the chemical environment of Pd is changed and part of electrons are lost.
Referring to FIG. 3, curves 1 and 2 are the O1s binding spectra of the ketone carbonyl and ester carbonyl oxygen atoms in the complex ring, respectively, with binding energies of 530.4 and 532.3eV, which are lower than the O1s standard binding energies of the ketone carbonyl and ester carbonyl oxygen atoms, because the carbonyl oxygen atoms gain part of the electrons of the palladium atom and thus their binding energies are reduced. Curves 3 and 4 are the O1s binding spectra for C-O-C and the carbonyl oxygen atom in the aliphatic chain, respectively, with no change in binding energy compared to the standard binding energy, and curve 5 is the superimposed peak of the O1s spectra in the three chemical environments. Further illustrates that the interaction between the heart-shaped nano palladium and the substrate P (AAEM-St) is the chemical force formed between the nano palladium particles and the carbonyl oxygen atoms in the long chain of the substrate.
Referring to fig. 4, the decomposition temperature of the P (AAEM-St) coated heart-shaped nano palladium particle composite material is significantly lower than that of P (AAEM-St), which may be due to the interaction force between two carbonyl oxygen atoms in the long chain of the substrate P (AAEM-St) and a palladium atom, which induces the palladium atom to agglomerate to form heart-shaped nano palladium particles, and the presence of the defect structure of the heart-shaped nano palladium particles makes the nano palladium particles have better thermal catalytic performance, which promotes the thermal degradation of the substrate P (AAEM-St).
Referring to fig. 5, it can be seen that four diffraction peaks appear at the diffraction angles 2 θ of 37.91 °, 44.14 °, 64.46 ° and 77.41 °, respectively, which are substantially consistent with the positions corresponding to the (PDFWIN #87-0637) (111), (200), (220) and (311) crystal planes of the palladium standard, indicating that the synthesized composite material contains nano-palladium particles and has a face-centered cubic structure.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. A preparation method of a P (AAEM-St) coated heart-shaped nano palladium particle composite material is characterized in that in the composite material, a P (AAEM-St) polymer induces nano palladium particles to form a heart-shaped structure;
the preparation method of the P (AAEM-St) coated heart-shaped nano palladium particle composite material comprises the following steps:
1) AAEM pretreatment: putting the AAEM into a separating funnel, washing the AAEM3-4 times by using deionized water, and putting the lower-layer liquid into a clean conical flask for later use;
2) weighing PdCl2, adding deionized water for dissolving once, then adding AAEM and styrene, adding deionized water for the second time, stirring uniformly, and then adding an initiator;
3) ultrasonic treatment: obtaining a reaction solution;
4) washing and drying: slowly pouring the reaction solution into a beaker filled with absolute ethyl alcohol, stirring while pouring, washing for many times until the product is changed into black powder from black flocculent precipitate, discarding the supernatant, naturally drying the remaining product, grinding and loading the product into a sample;
the addition ratio of the PdCl2, the primary deionized water, the AAEM, the styrene, the secondary deionized water and the initiator in the step 2) is 0.050g to 20mL to 1mL to 5mL to 30mL to 0.012 g;
the ultrasonic treatment condition in the step 3): working time is 40-60min, ultrasonic treatment is 1s, intermittence is 1s, power is 36%, and temperature is 40-45 ℃.
2. The method for preparing P (AAEM-St) coated nano palladium particle composite material according to claim 1, wherein the initiator in the step 2) is potassium persulfate or azobisisobutyronitrile.
3. P (AAEM-St) coated nano-palladium particle composites in heart shape prepared according to the method of claim 1 or 2.
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Citations (3)
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| CN102775548A (en) * | 2012-07-30 | 2012-11-14 | 安徽理工大学 | Method for polymerizing and preparing nanometer silver-PAAEM (Ploy Acetoacetoxyethyl Methacrylate) composite material through ultrasonically initiating emulsifier-free emulsion |
| CN102873334A (en) * | 2012-10-12 | 2013-01-16 | 安徽理工大学 | Ultrasonic radiation preparation method for chrysanthemum-like nano-palladium aggregate material |
| CN104347192A (en) * | 2014-10-17 | 2015-02-11 | 深圳市飞世尔实业有限公司 | Method for preparing electronic conductive micro-sphere for producing anisotropic conductive film by simply absorbing metal palladium ions |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102775548A (en) * | 2012-07-30 | 2012-11-14 | 安徽理工大学 | Method for polymerizing and preparing nanometer silver-PAAEM (Ploy Acetoacetoxyethyl Methacrylate) composite material through ultrasonically initiating emulsifier-free emulsion |
| CN102873334A (en) * | 2012-10-12 | 2013-01-16 | 安徽理工大学 | Ultrasonic radiation preparation method for chrysanthemum-like nano-palladium aggregate material |
| CN104347192A (en) * | 2014-10-17 | 2015-02-11 | 深圳市飞世尔实业有限公司 | Method for preparing electronic conductive micro-sphere for producing anisotropic conductive film by simply absorbing metal palladium ions |
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