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Poly-o-phenylenediamine nanometer metal composite particle and preparation method

A poly-o-phenylenediamine and nano-metal technology, applied in the direction of coating, etc., to achieve the effect of simple preparation method, high reproducibility, and short experimental cycle

Inactive Publication Date: 2014-12-17
ZHEJIANG UNIV
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Problems solved by technology

This nano-core-shell composite has not been reported in marine antifouling coatings

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  • Poly-o-phenylenediamine nanometer metal composite particle and preparation method

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[0031] 聚邻苯二胺-纳米金属复合颗粒的制备方法的步骤如下:

[0032] 1)在冰浴环境下,将0.002-0.006 mol金属硝酸盐溶解于20-80mL 质量百分比浓度为2%-8%的分散-稳定剂溶液中,使用机械搅拌使上述混合液发泡,发泡量为分散-稳定剂溶液体积的5倍,取0.001-0.005 mol还原剂溶解于冰水,待溶解完全后将还原剂溶液逐滴滴入金属硝酸盐-分散剂溶液中,使反应液中的金属离子完全转变为金属单质;

[0033] 2)上述反应完全后,将步骤1)中的反应液加入离心管,在2000 r / min转速下进行离心分离2-4 min,将所得胶体金属稀释100倍后作紫外分析,验证纳米金属颗粒 Synthesis;

[0034] 3)取0.0005-0.0015 mol邻苯二胺加入至1mol / L的盐酸溶液中,超声处理使其完全溶解,取等体积的邻苯二胺盐酸溶液与胶体金属混合,搅拌12小时使邻苯二胺上的氨基与纳米金属颗粒结合并分散均匀;

[0035] 4)将氧化剂溶于水,然后在冰浴条件下,将氧化剂溶液逐滴滴加至步骤3)所得到的溶液,搅拌使其反应18-24个小时;

[0036] 5)脱水后淋洗,得到聚邻苯二胺-纳米金属复合颗粒。

[0037] 所述的金属硝酸盐是硝酸铜、硝酸银或硝酸铋。所述的分散-稳定剂是聚乙烯醇,聚乙二醇或聚乙烯吡咯烷酮中的一种或数种。所述的还原剂是硼氢化钠,所述的氧化剂是过硫酸铵。所述的脱水是离心脱水、压滤脱水或抽滤脱水。所述的胶体金属的分散剂是质量百分比浓度为2-8%的分散剂水溶液20-80mL。

[0038] 本发明的纳米金属颗粒及其尺寸通过紫外-可见分光光度计(uv-vis)及透射电子显微镜(TEM)证实,本发明的聚邻苯二胺-纳米金属颗粒核壳结构通过透射电子显微镜(TEM)及能量色散X射线光谱仪(EDX)证实。

Embodiment 1

[0040] 1)在冰浴环境下,将0.002mol硝酸铜溶解于20mL 8%的聚乙烯醇溶液中。使用强机械搅拌使上述混合液发泡,发泡量为聚乙烯醇分散-稳定剂溶液体积的5倍。取0.001mol硼氢化钠溶解于冰水。待溶解完全后将硼氢化钠溶液逐滴滴入硝酸铜-聚乙烯醇溶液中,使反应液中的铜离子完全转变为铜单质。

[0041] 2)上述反应完全后,将步骤1)中的反应液加入至离心管,在2000 r / min转速下进行离心分离2 min,将所得胶体金属稀释100倍后作紫外分析,验证纳米铜颗粒的 synthesis;

[0042] 3)取0.0005 mol邻苯二胺加入至1mol / L的盐酸溶液中,超声处理使其完全溶解,取等体积的邻苯二胺盐酸溶液与胶体金属混合,搅拌12小时使邻苯二胺上的氨基与纳米铜颗粒结合并分散均匀;

[0043] 4)将过硫酸铵溶于水,然后在冰浴条件下,将过硫酸铵溶液逐滴滴加至3)所得到的溶液。搅拌使其反应18个小时;

[0044] 5)脱水后淋洗,得到聚邻苯二胺-纳米铜复合颗粒。

Embodiment 2

[0046]1) Dissolve 0.004 mol silver nitrate in 40mL 4% polyethylene glycol solution in an ice bath environment. Use strong mechanical stirring to make the above mixed solution foam, and the foaming amount is 5 times the volume of the polyethylene glycol dispersion-stabilizer solution. Take 0.001 mol sodium borohydride dissolved in ice water. After the dissolution is complete, the sodium borohydride solution is dropped dropwise into the silver nitrate-polyethylene glycol solution, so that the silver ions in the reaction solution are completely converted into simple silver.

[0047] 2) After the above reaction is complete, add the reaction solution in step 1) to the centrifuge tube, and perform centrifugation at 2000 r / min for 3 minutes, dilute the obtained colloidal metal 100 times, and then conduct ultraviolet analysis to verify the concentration of silver nanoparticles. synthesis;

[0048] 3) Take 0.001mol o-phenylenediamine and add it to 1mol / L hydrochloric acid solution, s...

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Abstract

The invention discloses a poly-o-phenylenediamine nanometer metal composite particle and a preparation method. The poly-o-phenylenediamine nanometer metal composite particle has a nuclear shell self-assembly structure. The preparation method comprises the steps that nanometer metal particles are produced through metal salt under the protection of dispersion-stabilizer by taking sodium borohydride as the reducing agent; the surface layer of the nanometer metal particle is bonded stably with the amidogen of o-phenylenediamine; the solution polymerization of o-phenylenediamine is then triggered with ammonium persulfate as the oxidant, so that the poly-o-phenylenediamine nanometer metal composite particle is obtained. The core of the composite particle is nanometer metal, and the shell of the composite particle is amidogen grafted polyaniline; the sterilization property of the nanometer metal and the biotoxicity of polyaniline realizes synergistic effect, meanwhile, polyaniline is insoluble in water, and the environmental safety of antibacterial powder is improved. The poly-o-phenylenediamine nanometer metal composite particle and the preparation method have the advantages that the specific surface is large, the antibiosis range is large, the sterilization effect is durable, the conductivity is high and stable, the service life is long, the composite particle can be used as antiseptic agent and antifouling additive, and is particularly suitable for marine antiseptic antifouling paint.

Description

technical field [0001] The invention relates to a poly-o-phenylenediamine-nanometer metal composite particle and a preparation method. Background technique [0002] Common antifouling coatings are mainly composed of resins, antifouling agents, auxiliary materials, fillers and solvents. After forming a coating film on the metal surface, it is an antifouling coating. As the mainstay of antifouling coatings, in the 1970s, organic tin (TBT) acrylic resin self-polishing composites had an antifouling validity period of more than 5 years and the characteristics of keeping the bottom of the ship smooth. However, organotin coatings have caused significant damage to the marine ecological environment and can endanger human health through the food chain. Finding an environment-friendly marine antifouling coating has become a technical problem to be solved urgently. [0003] In recent years, it has been reported that marine corrosion originates from microorganisms, and the metabolites ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/02
Inventor 赵国辰黄元凤秦文莉叶瑛裘林莉
Owner ZHEJIANG UNIV
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