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A method for preparing 3-methylthiophene-coated nano-particle magnetic nickel zinc ferrite liquid polyethylene

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CN103632798B
CN103632798B CN 201310636021 CN201310636021A CN103632798B CN 103632798 B CN103632798 B CN 103632798B CN 201310636021 CN201310636021 CN 201310636021 CN 201310636021 A CN201310636021 A CN 201310636021A CN 103632798 B CN103632798 B CN 103632798B
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CN 201310636021
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CN103632798A (en )
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乐长高
谢宇
潘建飞
谢宗波
黄彦
李凤
刘福明
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东华理工大学
南昌航空大学
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Abstract

本发明公开了一种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体的制备方法,通过表面原位合成法将镍锌铁氧体粒子用聚3-甲基噻吩包覆,达到聚3-甲基噻吩牢固包裹镍锌铁氧体纳米颗粒的效果,具体采用共沉淀法先制备镍锌铁氧体纳米颗粒,随后用所制得镍锌铁氧体纳米颗粒制备镍锌铁氧体离子型磁性液体,再在镍锌铁氧体离子型磁性液体中加入3-甲基噻吩单体和引发剂原位聚合得到聚3-甲基噻吩良好包覆纳米镍锌铁氧体磁性粒子,最后用镍锌铁氧体/聚3-甲基噻吩复合颗粒制备出聚3-甲基噻吩包覆纳米镍锌铁氧体磁性粒子磁性液体。 The present invention discloses a poly-3-methylthiophene preparing nano nickel zinc ferrite particles coated with a magnetic fluid, the surface of the in situ synthesis method by nickel zinc ferrite particles were coated with poly-3-methylthiophene, achieve the effect of poly-3-methylthiophene securely wrapped nickel zinc ferrite nanoparticles, particularly to nickel zinc ferrite nanoparticles prepared by coprecipitation, followed by nickel zinc ferrite prepared Nanocrystalline nickel-zinc iron particles ionic liquids magnetic ferrite, Ni-Zn ferrite was further added in an ionic magnetic liquid 3-methylthiophene-situ polymerization of the monomers and initiator to obtain poly-3-methylthiophene good magnetic nickel zinc ferrite coated nano particles, and finally nickel zinc ferrite / poly 3-methylthiophene composite particles prepared a poly 3-methylthiophene coated nano nickel zinc ferrite magnetic particles magnetic liquid.

Description

一种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体的制备方法 A method for preparing 3-methylthiophene-coated nano-particle magnetic nickel zinc ferrite liquid polyethylene

技术领域 FIELD

[0001] 本发明涉及一种导电聚合物包裹纳米磁性颗粒磁性液体的制备方法,尤其涉及一种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体的制备方法。 [0001] The present invention relates to a method for wrapping a magnetic liquid nanomagnetic particles a conductive polymer, particularly to a method for preparing 3-methylthiophene-coated nano-particle magnetic nickel zinc ferrite liquid polyethylene.

背景技术 Background technique

[0002] 磁性液体是指尺寸量级小于单磁畴的纳米磁性颗粒高度弥散于液态基载液中而构成的一种高稳定性的胶体溶液,一般的磁性液体的分散剂是有机高分子链,不具备特殊的性能,而磁性液体中一旦在原先的纳米磁性颗粒和分散剂衔接处包裹上一层有机半导体后,一种新型的有机无机杂化磁性液体便应运而生,有机半导体通过与磁性液体有机结合后,有机半导体的性能便可通过调节磁场强度来使磁性液体具备规律性的光电性能变化, 因此该类新型磁性液体在微光器件和光子晶体等领域的应用上具有巨大潜力。 [0002] The magnetic order of magnitude less than the liquid means monodomain nanomagnetic particles highly dispersed in a liquid-based carrier liquid to form a colloidal solution having high stability, a dispersant is generally an organic liquid of magnetic polymer chain , do not have the specific properties, and the magnetic fluid on the package once the nanomagnetic particles and the dispersant at the convergence of the original organic semiconductor layer, a new organic-inorganic hybrid magnetic fluid have come into being, through an organic semiconductor after the combination of the magnetic fluid, the performance of the organic semiconductor can be provided with the magnetic fluid regular optical properties varied by adjusting the magnetic field strength, the magnetic fluid having a novel class great potential in the field of photonic crystal devices and the like shimmer on the application.

[0003] 但是这类磁性液体的制备需要克服三个难点:一是导电聚3-甲基噻吩包裹磁性纳米铁氧体颗粒的稳定性;二是导电聚3-甲基噻吩包裹层的尺寸量级控制;三是包裹后的纳米磁性颗粒如何稳定分散于基载液中。 [0003] However, the preparation of such a magnetic liquid to overcome three difficulties: First, stability of the conductive poly-3-methylthiophene magnetic nanoparticles wrapped ferrite particles; two dimensional quantity of conductive poly 3-methylthiophene wrapping layer level control; Third, after wrapping nanomagnetic particles dispersed in the matrix how to stabilize the carrier liquid.

发明内容 SUMMARY

[0004] 本发明的目的是提供一种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体的制备方法,提高了导电聚3-甲基噻吩包裹磁性纳米铁氧体颗粒的稳定性,控制了导电聚3-甲基噻吩包裹层的尺寸量级,使得包裹后的纳米磁性颗粒稳定分散于基载液中。 [0004] The object of the present invention is to provide a poly-3-methylthiophene-coated nano-particles prepared nickel zinc ferrite magnetic fluid, improve the stability of the conductive poly-3-methylthiophene magnetic nanoparticles wrapped ferrite particles , control the order of the size of the conductive poly-3-methylthiophene wrap layer, such that a stable nanomagnetic particles dispersed in the matrix after wrapping the carrier liquid.

[0005] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0005] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0006] A、把31. 32g Fe(NO3)3 ·9Η20、12· 89g Ni (NO3)2 ·6Η20、24· 57g Zn(NO3)2 ·6Η20溶解于250ml水中配置成溶液,再把12. 24g FeSO4 · 7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌20-30分钟,然后磁分离4-6小时,用去离子水洗涤至ρΗ=7· 0,把82. 02g Fe(NO3)3 ·9Η20溶解于500ml水中配置成Fe(NO3)3 ·9Η20 溶液,把Fe (NO3) 3 · 9Η20溶液倒入洗涤好的上述溶液中沸腾30-40分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉,即得纳米镍锌铁氧体粒子; [0006] A, the 31. 32g Fe (NO3) 3 · 9Η20,12 · 89g Ni (NO3) 2 · 6Η20,24 · 57g Zn (NO3) 2 · 6Η20 configured dissolved in 250ml of water to the solution, and then 12. 24g FeSO4 · 7Η20 configured dissolved in 250ml of water as a solution, the solution was poured into two or more concentrated aqueous ammonia was added after 70 mL three-neck flask was dissolved and stirred for 20-30 minutes, 4-6 hours and then magnetically separated, washed with deionized water to ρΗ = 7 · 0, the 82. 02g Fe (NO3) 3 · 9Η20 configured dissolved in 500ml of water to Fe (NO3) 3 · 9Η20 solution, washing was poured into the Fe (NO3) 3 · 9Η20 a good solution to the solution boiling 30-40 minutes, magnetically separated to cool to room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain particles of nano nickel zinc ferrite ;

[0007] Β、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成1-2%的镍锌铁氧体Massart磁性液体,熟化6-8天; [0007] Β, 5g of the above step was nano nickel zinc ferrite particles was added 94. 47ml0. 91 mol. L 1 is dubbed nitrate solution of 1-2% nickel zinc ferrite magnetic fluid Massart, aged 6 -8 days;

[0008] C、在烧杯中加入已制备好的Massart磁性液体加水100mL稀释混合均匀后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴3-4h,并在期间加入15%过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8mol/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0008] C, has been added in a beaker prepared Massart 100mL magnetic liquid was diluted with water after mixing uniformly, the 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and Ig sulfanilic acid added to the beaker in an ice-water bath after 3-4h, and was added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0. 8mol / l of sulfuric acid and acetone, washed with acetone until PH = 7, Ni - Zn ferrite / poly 3-methylthiophene composite particles;

[0009] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应24-26h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0009] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 24-26h, could not be removed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methyl thiophene-nickel-zinc ferrite particles coated nano magnetic fluid.

[0010] 本发明的优点是:本发明通过表面原位合成法将纳米镍锌铁氧体粒子用聚3-甲基噻吩包覆,达到聚3-甲基噻吩牢固包裹镍锌铁氧体纳米颗粒的效果,通过数学计算3-甲基噻吩单体数量,再辅以阻聚剂精确控制聚合度,防止3-甲基噻吩聚合度超过磁性液体所能承载的尺寸量级,控制在10-20纳米,从而达到控制镍锌铁氧体/聚3-甲基噻吩复合颗粒粒径的效果,获得磁性液体,同时也提高了导电聚3-甲基噻吩包裹磁性纳米铁氧体颗粒的稳定性(放置六个月不下沉)。 [0010] The advantage of the present invention are: the present invention, nano nickel zinc ferrite particles were coated with poly-3-methylthiophene-situ synthesis by a surface, to poly-3-methylthiophene securely wrapped nickel zinc ferrite nano the effect of the particle, the number of 3-methylthiophene mathematically monomer, a polymerization inhibitor supplemented precise control of polymerization degree, preventing the degree of polymerization of 3-methyl-thiophene order of magnitude more than can carry a magnetic liquid, controlled 10- 20 nm, so as to control the Ni-Zn ferrite / poly 3-methylthiophene composite effect of particle size, the magnetic fluid is obtained, but also improve the stability of the conductive poly-3-methylthiophene magnetic nanoparticles wrapped ferrite particles (placed for six months does not sink). 该磁性液体由于有一层导电聚合物包覆层,因此其在规律性变化磁场作用下,其光电性能方面产生亦能的规律性变化,即最终达到通过调节磁场强度可控调节其在光电方面的性能指标的目的,在磁性液体的研究中开辟出了一个新颖的可供研究的小分支,具有很重要的研究及应用价值。 Since the magnetic layer of a conductive polymer liquid clad layer, its magnetic field at regular changes, which can also produce photovoltaic performance of regular change, i.e., ultimately controlled by adjusting the magnetic field intensity is adjusted in terms of the photoelectric the purpose of performance indicators, to open up the study of magnetic fluid in a small branch of research for a novel, and have important research value.

具体实施方式 detailed description

[0011] 结合上述发明内容提供以下实施案例。 [0011] The invention provides the following in conjunction with the above embodiments cases.

[0012] 实施例1 : [0012] Example 1:

[0013] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0013] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0014] A、把31.32g Fe(N03)3.9H20、12.89g Ni(N03)2.6H20、24.57g Ζη(Ν03)2·6Η20 溶解于250ml水中配置成溶液,再把12. 24g FeSO4 ·7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌20分钟,然后磁分离4小时,用去离子水洗涤至pH=7. 0,把82. 02g Fe (NO3) 3 · 9H20溶解于500ml水中配置成Fe (NO3) 3 · 9H20 溶液,把Fe (NO3) 3 · 9H20溶液倒入洗涤好的上述溶液中沸腾30分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉, 即得纳米镍锌铁氧体粒子; [0014] A, the 31.32g Fe (N03) 3.9H20,12.89g Ni (N03) 2.6H20,24.57g Ζη (Ν03) 2 · 6Η20 was dissolved in 250ml of water was arranged, and then dissolving 12. 24g FeSO4 · 7Η20 arranged in 250ml water solution, the solution was poured into two or more concentrated aqueous ammonia was added 70 mL three-neck flask was dissolved after stirring for 20 minutes, then magnetic separation for 4 hours and washed with deionized water until pH = 7. 0, to 82. 02g Fe (NO3) 3 · 9H20 were dissolved in 500ml of water disposed to Fe (NO3) 3 · 9H20 solution of the Fe (NO3) 3 · 9H20 solution was poured into the above solution was washed well boiled for 30 minutes to be cooled to a magnetic separation at room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain nano nickel zinc ferrite particles;

[0015] B、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成1%的镍锌铁氧体Massart磁性液体,熟化6天; [0015] B, 5g of the above step was nano nickel zinc ferrite particles 94. 47ml0 91 mol of nitric acid was added a solution of L 1 to form 1% nickel zinc ferrite magnetic fluid Massart, aged for 6 days..;

[0016] C、在烧杯中加入已制备好的Massart磁性液体加水100mL稀释混合均勾后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴3h,并在期间加入15% 过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8m〇l/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0016] C, has been added in a beaker Massart good magnetic fluid prepared by adding water after mixing were diluted with 100mL hook, will 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and sulfanilic Ig into a beaker of ice water bath for 3h, and was added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0.1 8m〇l / l sulfuric acid, and acetone and then washed with acetone to PH = 7, Ni - Zn ferrite body / poly 3-methylthiophene composite particles;

[0017] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应24h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0017] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 24h, it failed to remove the Ni-Zn ferrite is uniformly dispersed with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methylthiophene package nano-particles coated nickel zinc ferrite magnetic fluid.

[0018] 实施例2 : [0018] Example 2:

[0019] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0019] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0020] A、把31.32g Fe(N03)3.9H20、12.89g Ni(N03)2.6H20、24.57g Ζη(Ν03)2·6Η20 溶解于250ml水中配置成溶液,再把12. 24g FeSO4 ·7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌25分钟,然后磁分离5小时,用去离子水洗涤至pH=7. 0,把82. 02g Fe (NO3) 3 · 9H20溶解于500ml水中配置成Fe (NO3) 3 · 9H20 溶液,把Fe (NO3) 3 · 9H20溶液倒入洗涤好的上述溶液中沸腾35分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉, 即得纳米镍锌铁氧体粒子; [0020] A, the 31.32g Fe (N03) 3.9H20,12.89g Ni (N03) 2.6H20,24.57g Ζη (Ν03) 2 · 6Η20 was dissolved in 250ml of water was arranged, and then dissolving 12. 24g FeSO4 · 7Η20 arranged in 250ml water solution, the solution was poured into two or more concentrated aqueous ammonia was added after 70 mL three-neck flask was dissolved and stirred for 25 minutes, then magnetic separation for 5 hours and washed with deionized water until pH = 7. 0, to 82. 02g Fe (NO3) 3 · 9H20 were dissolved in 500ml of water disposed to Fe (NO3) 3 · 9H20 solution of the Fe (NO3) 3 · 9H20 solution was poured into the above solution was washed well boiled for 35 minutes to be cooled to a magnetic separation at room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain nano nickel zinc ferrite particles;

[0021] B、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成1. 5%的镍锌铁氧体Massart磁性液体,熟化6-8天; [0021] B, above 5g step nano nickel zinc ferrite particles obtained by adding 94. 47ml0. 91 mol. L 1 is dubbed nitrate solution of 1.5% nickel zinc ferrite magnetic fluid Massart, aged 6 -8 days;

[0022] C、在烧杯中加入已制备好的Massart磁性液体加水100mL稀释混合均匀后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴3. 5h,并在期间加入15%过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8mol/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0022] C, has been added in a beaker prepared Massart 100mL magnetic liquid was diluted with water after mixing uniformly, the 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and Ig sulfanilic acid added to the beaker in an ice-water bath after 3. 5h, and was added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0. 8mol / l of sulfuric acid and acetone, washed with acetone until PH = 7, Ni - Zn ferrite / poly 3-methylthiophene composite particles;

[0023] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应25h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0023] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 25H, could not be removed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methylthiophene package nano-particles coated nickel zinc ferrite magnetic fluid.

[0024] 实施例3 : [0024] Example 3:

[0025] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0025] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0026] A、把31.32g Fe(N03)3.9H20、12.89g Ni(N03)2.6H20、24.57g Ζη(Ν03)2·6Η20 溶解于250ml水中配置成溶液,再把12. 24g FeSO4 ·7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌30分钟,然后磁分离6小时,用去离子水洗涤至pH=7. 0,把82. 02g Fe (NO3) 3 · 9H20溶解于500ml水中配置成Fe (NO3) 3 · 9H20 溶液,把Fe (NO3) 3 · 9H20溶液倒入洗涤好的上述溶液中沸腾40分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉, 即得纳米镍锌铁氧体粒子; [0026] A, the 31.32g Fe (N03) 3.9H20,12.89g Ni (N03) 2.6H20,24.57g Ζη (Ν03) 2 · 6Η20 was dissolved in 250ml of water was arranged, and then dissolving 12. 24g FeSO4 · 7Η20 arranged in 250ml water solution, the solution was poured into two or more concentrated aqueous ammonia was added 70 mL three-neck flask was dissolved after stirring for 30 minutes, 6 hours and then magnetically separated, washed with deionized water until pH = 7. 0, to 82. 02g Fe (NO3) 3 · 9H20 were dissolved in 500ml of water disposed to Fe (NO3) 3 · 9H20 solution of the Fe (NO3) 3 · 9H20 solution was poured into the above solution was washed well boiled for 40 minutes to be cooled to a magnetic separation at room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain nano nickel zinc ferrite particles;

[0027] B、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成2%的镍锌铁氧体Massart磁性液体,熟化8天; [0027] B, above 5g step nano nickel zinc ferrite particles obtained by adding 94. 47ml0 91 mol L dubbed nitrate solution 1 2% Ni-Zn ferrite magnetic fluid Massart, aged 8 days..;

[0028] C、在烧杯中加入已制备好的Massart磁性液体加水100mL稀释混合均匀后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴4h,并在期间加入15% 过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8m〇l/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0028] C, has been added in a beaker prepared Massart 100mL magnetic liquid was diluted with water after mixing uniformly, the 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and Ig sulfanilic acid added to the beaker in an ice-water bath after 4h, and added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0.1 8m〇l / l of sulfuric acid and acetone, washed with acetone until PH = 7, Ni - Zn ferrite / poly 3-methylthiophene composite particles;

[0029] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应26h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0029] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature 26h is, could not be removed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methylthiophene package nano-particles coated nickel zinc ferrite magnetic fluid.

[0030] 实施例4 : [0030] Example 4:

[0031 ] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0031] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0032] A、把31.32g Fe(N03)3.9H20、12.89g Ni(N03)2.6H20、24.57g Ζη(Ν03)2·6Η20 溶解于250ml水中配置成溶液,再把12. 24g FeSO4 ·7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌18分钟,然后磁分离3小时,用去离子水洗涤至pH=7. 0,把82. 02g Fe (NO3) 3 · 9H20溶解于500ml水中配置成Fe (NO3) 3 · 9H20 溶液,把Fe (NO3) 3 · 9H20溶液倒入洗涤好的上述溶液中沸腾25分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉, 即得纳米镍锌铁氧体粒子; [0032] A, the 31.32g Fe (N03) 3.9H20,12.89g Ni (N03) 2.6H20,24.57g Ζη (Ν03) 2 · 6Η20 was dissolved in 250ml of water was arranged, and then dissolving 12. 24g FeSO4 · 7Η20 arranged in 250ml water solution, the solution was poured into two or more concentrated aqueous ammonia was added after 70 mL three-neck flask was dissolved and stirred for 18 minutes and then magnetically separated for 3 hours and washed with deionized water until pH = 7. 0, to 82. 02g Fe (NO3) 3 · 9H20 were dissolved in 500ml of water disposed to Fe (NO3) 3 · 9H20 solution of the Fe (NO3) 3 · 9H20 solution was poured into the above solution was washed well boiled for 25 minutes to be cooled to a magnetic separation at room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain nano nickel zinc ferrite particles;

[0033] B、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成1%的镍锌铁氧体Massart磁性液体,熟化6-8天; [0033] B, above 5g step nano nickel zinc ferrite particles obtained by adding 94. 47ml0. 91 mol. L nitrate solution to form 1 1% of the Ni-Zn ferrite magnetic fluid Massart, aged 6-8 day;

[0034] C、在烧杯中加入已制备好的Massart磁性液体加水100mL稀释混合均匀后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴2h,并在期间加入15% 过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8m〇l/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0034] C, has been added in a beaker prepared Massart 100mL magnetic liquid was diluted with water after mixing uniformly, the 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and Ig sulfanilic acid added to the beaker in an ice-water bath after 2h, and was added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0.1 8m〇l / l of sulfuric acid and acetone, washed with acetone until PH = 7, Ni - Zn ferrite / poly 3-methylthiophene composite particles;

[0035] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应20h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0035] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 20 h, remove failed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methylthiophene package nano-particles coated nickel zinc ferrite magnetic fluid.

[0036] 实施例5 : [0036] Example 5:

[0037] -种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体,其制备方法为: [0037] - poly 3-methylthiophene species nano nickel zinc ferrite particles coated with a magnetic fluid, which is prepared as follows:

[0038] A、把31.32g Fe(N03)3.9H20、12.89g Ni(N03)2.6H20、24.57g Ζη(Ν03)2·6Η20 溶解于250ml水中配置成溶液,再把12. 24g FeSO4 ·7Η20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70 mL浓氨水,搅拌35分钟,然后磁分离7小时,用去离子水洗涤至pH=7. 0,把82. 02g Fe (NO3) 3 · 9H20溶解于500ml水中配置成Fe (NO3) 3 · 9H20 溶液,把Fe (NO3) 3 · 9H20溶液倒入洗涤好的上述溶液中沸腾45分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉, 即得纳米镍锌铁氧体粒子; [0038] A, the 31.32g Fe (N03) 3.9H20,12.89g Ni (N03) 2.6H20,24.57g Ζη (Ν03) 2 · 6Η20 was dissolved in 250ml of water was arranged, and then dissolving 12. 24g FeSO4 · 7Η20 arranged in 250ml water solution, the solution was poured into two or more concentrated aqueous ammonia was added after 70 mL three-necked flask to dissolve, stirred for 35 minutes, then magnetic separation 7 hours, washed with deionized water until pH = 7. 0, to 82. 02g Fe (NO3) 3 · 9H20 were dissolved in 500ml of water disposed to Fe (NO3) 3 · 9H20 solution of the Fe (NO3) 3 · 9H20 solution was poured into the above solution was washed well boiled for 45 minutes to be cooled to a magnetic separation at room temperature, the supernatant was drained, washed repeatedly with deionized water until neutral, dried in a vacuum NATURAL dish, pulverized to obtain nano nickel zinc ferrite particles;

[0039] B、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91 mol. L 1的硝酸溶液配成2%的镍锌铁氧体Massart磁性液体,熟化6-8天; [0039] B, above 5g step nano nickel zinc ferrite particles obtained by adding 94. 47ml0. 91 mol. L solution of nitric acid 1 dubbed 2% Ni-Zn ferrite magnetic fluid Massart, aged 6-8 day;

[0040] C、在烧杯中加入已制备好的Mas sart磁性液体加水I OOml稀释混合均匀后,将3ml 3-甲基噻吩、0. 8ml硫酸和Ig无水对氨基苯磺酸加入烧杯中,冰水浴5h,并在期间加入15% 过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8m〇l/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; [0040] C, Mas sart good magnetic fluid was prepared in a beaker was added after dilution with water I OOml mixed, the 3ml 3- methylthiophene, 0. 8ml of anhydrous sulfuric acid and Ig sulfanilic acid added to the beaker, ice-water bath 5h, and was added during a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0.1 8m〇l / l sulfuric acid, and acetone and then washed with acetone to PH = 7, Ni - Zn - Fe ferrite / poly 3-methylthiophene composite particles;

[0041] D、取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. Sg十六烷基苯磺酸钠、2ml 90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应28h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 [0041] D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. Sg hexadecyl benzene sulfonate, 2ml 90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 28H, could not be removed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methylthiophene package nano-particles coated nickel zinc ferrite magnetic fluid.

[0042] 各个实施例制得的聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体性能如下表所示: [0042] each coated nano nickel zinc ferrite magnetic particles prepared in Example performance liquid poly 3-methylthiophene embodiment shown in the following table:

[0043] [0043]

Figure CN103632798BD00071

[0044] 从以上数据可以看出,在本发明工艺范围内的实施例1-3制得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体所能承载的尺寸量级,控制在10-20纳米,温度性良好,明显优于在本发明工艺范围外的实施例4、5,可见采用了本发明制备的聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体性能具有良好的尺寸量级和稳定性,有重要的应用价值。 [0044] As can be seen from the above data, the process embodiments within the scope of the present invention 1-3 order of magnitude to obtain poly-3-methylthiophene-coated nano nickel zinc ferrite magnetic particles can carry a liquid, the control 10-20 nm, temperature good, much better than in Examples 4 and 5 outside the scope of the process of the present invention, seen using poly 3-methylthiophene according to the present invention is prepared by coating nano-particle magnetic nickel zinc ferrite liquid performance has good dimensional stability and order of magnitude, there is great value.

Claims (1)

1. 一种聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体的制备方法,其特征为: 其制备方法为: A、把31. 32gFe(N03)3 · 9Η20、12· 89gNi(N03)2 · 6Η20、24· 57gΖη(Ν03)2 · 6H20 溶解于250ml水中配置成溶液,再把12. 24gFeS04 · 7H20溶解于250ml水中配置成溶液,把以上两种溶液倒入三口烧瓶中溶解后加入70mL浓氨水,搅拌20-30分钟,然后磁分离4-6小时,用去离子水洗涤至ρΗ=7· 0,把82. 02gFe(N03)3 ·9Η20溶解于500ml水中配置成Fe(N03)3 ·9Η20 溶液,把Fe(Ν03) 3 · 9Η20溶液倒入洗涤好的上述溶液中沸腾30-40分钟,磁分离至自然冷却至室温,倒掉上层清液,用去离子水反复洗涤直至中性,在真空干燥皿中自然干燥,研磨成粉,即得纳米镍锌铁氧体粒子; Β、取5克上述步骤所得纳米镍锌铁氧体粒子,加入94. 47ml0. 91mol.L1的硝酸溶液配成1-2%的镍锌铁氧体Massart磁性液体,熟化6-8天; C、 在烧 1. A method for the preparation of poly-3-methylthiophene-coated nano nickel zinc ferrite magnetic particles in a liquid, wherein: Method of preparation: A, the 31. 32gFe (N03) 3 · 9Η20,12 · 89gNi (N03) 2 · 6Η20,24 · 57gΖη (Ν03) 2 · 6H20 dissolved in 250ml of water was arranged, and then 12. 24gFeS04 · 7H20 dissolved in 250ml of water arranged as a solution, the solution was poured into two or more three-necked flask was dissolved after addition of 70mL of concentrated aqueous ammonia, stirred for 20-30 minutes, 4-6 hours and then magnetically separated, washed with deionized water until ρΗ = 7 · 0, the 82. 02gFe (N03) 3 · 9Η20 arranged in 500ml of water was dissolved Fe ( N03) 3 · 9Η20 solution, the Fe (Ν03) 3 · 9Η20 the washed solution was poured into the solution boiled for 30-40 minutes, magnetically separated to cool to room temperature, the supernatant was drained, washed with deionized water repeatedly and until neutral, and dried in vacuo to natural drying dish, pulverized to obtain nano-nickel-zinc ferrite particles; Beta, 5g of the above-described steps nano nickel zinc ferrite particles obtained by adding 94. 47ml0 91mol.L1. dubbed 1-2% nitric acid solution of nickel zinc ferrite magnetic fluid Massart, aged 6-8 days; C, burning 杯中加入已制备好的Massart磁性液体加水100ml稀释混合均勾后,将3ml3-甲基噻吩、0. 8ml硫酸和lg无水对氨基苯磺酸加入烧杯中,冰水浴3-4h,并在期间加入15%过硫酸铵溶液20ml,反应结束后磁分离,并用0. 8mol/l硫酸和丙酮各洗三次后,用丙酮洗涤至PH=7,得镍锌铁氧体/聚3-甲基噻吩复合粒子; D、 取1克制备好的镍锌铁氧体/聚3-甲基噻吩复合粒子加入到有0. 8g十六烷基苯磺酸钠、2ml90%乙醇和8ml去离子水的混合溶液中,室温下搅拌反应24-26h后,用高速离心机离心去除未能均匀分散的镍锌铁氧体/聚3-甲基噻吩复合粒子,取其上层液即得聚3-甲基噻吩包覆纳米镍锌铁氧体粒子磁性液体。 After the addition of a good cup of liquid was prepared Massart magnetic diluted with water 100ml were mixed hook, the 3ml3- methylthiophene, 0. 8ml lg of anhydrous sulfuric acid and sulfanilic acid added to the beaker in an ice-water bath 3-4h, and during the addition of a 15% ammonium persulfate solution 20ml, magnetic separation after the reaction, and washed three times each with 0. 8mol / l of sulfuric acid and acetone, washed with acetone until PH = 7, Ni - Zn ferrite / poly-3-methyl thiophene composite particles; D, taking 1 g prepared nickel zinc ferrite / poly 3-methylthiophene was added to the composite particles have 0. 8g hexadecyl benzene sulfonate, 2ml90% ethanol and deionized water 8ml the mixed solution, the reaction was stirred at room temperature for 24-26h, could not be removed uniformly dispersed nickel zinc ferrite with a high speed centrifuge / poly 3-methylthiophene composite particles, whichever supernatant to obtain poly-3-methyl thiophene-nickel-zinc ferrite particles coated nano magnetic fluid.
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