CN105399879B - A kind of preparation method of water-soluble Properties of Polystyrene Nano Particles - Google Patents
A kind of preparation method of water-soluble Properties of Polystyrene Nano Particles Download PDFInfo
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- 239000004793 Polystyrene Substances 0.000 title claims abstract description 31
- 229920002223 polystyrene Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 title description 11
- 239000004005 microsphere Substances 0.000 claims abstract description 27
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000005855 radiation Effects 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 8
- 239000010941 cobalt Substances 0.000 claims abstract description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000004132 cross linking Methods 0.000 claims abstract description 5
- 238000010894 electron beam technology Methods 0.000 claims abstract description 4
- 239000012467 final product Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 15
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 238000007720 emulsion polymerization reaction Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000012674 dispersion polymerization Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010557 suspension polymerization reaction Methods 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 230000004520 agglutination Effects 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
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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
- C08F112/00—Homopolymers 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
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/54—Polymerisation initiated by wave energy or particle radiation by X-rays or electrons
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Abstract
本发明属于高分子材料制备技术领域，尤其涉及一种水溶性聚苯乙烯纳米微球的制备方法，包括以下步骤：(1)将苯乙烯单体与去离子水混合，配制出A混合液；(2)将A混合液置于辐照容器中密封，通入氮气，然后利用钴源或电子束进行辐照交联，获得产物，将产物冷冻干燥或真空干燥获得最终产品，本方法采用辐射一步法制备水溶性聚苯乙烯纳米微球，合成方法快速简单、成本低廉、产量大、合成的聚苯乙烯微球能很好的溶于水。
The invention belongs to the technical field of polymer material preparation, and in particular relates to a method for preparing water-soluble polystyrene nano-microspheres, comprising the following steps: (1) mixing styrene monomers with deionized water to prepare a mixed solution of A; (2) Put the mixed solution A in an irradiation container and seal it, pass nitrogen gas into it, and then use cobalt source or electron beam to carry out irradiation crosslinking to obtain the product, and freeze-dry or vacuum-dry the product to obtain the final product. This method uses radiation The water-soluble polystyrene nanometer microsphere is prepared by one-step method, the synthesis method is fast and simple, the cost is low, the output is large, and the synthesized polystyrene microsphere can be well dissolved in water.
Description
技术领域technical field
本发明属于高分子材料制备技术领域，尤其涉及一种水溶性聚苯乙烯纳米微球的制备方法。The invention belongs to the technical field of polymer material preparation, and in particular relates to a preparation method of water-soluble polystyrene nano-microspheres.
背景技术Background technique
聚苯乙烯微球具有比表面积大、吸附性强、凝集作用大及表面反应能力强和易回收等特性。聚苯乙烯微球小的粒子尺寸和体积，使得整个粒子作为微反应器时对外界刺激具有响应性快和反应速率高的特性，大的比表面积可作为吸附、脱附、化学反应和光散射的反应位置，通常1g的尺寸为100nm的聚苯乙烯微球粒子提供有数十平方米到数百平方米的表面积。Polystyrene microspheres have the characteristics of large specific surface area, strong adsorption, strong agglutination, strong surface reaction ability and easy recovery. The small particle size and volume of polystyrene microspheres make the whole particle have the characteristics of fast response and high reaction rate to external stimuli when used as a microreactor, and the large specific surface area can be used as a substrate for adsorption, desorption, chemical reaction and light scattering. For the reaction site, usually 1 g of polystyrene microsphere particles with a size of 100 nm provides a surface area of tens of square meters to hundreds of square meters.
现在制备聚苯乙烯微球的途径主要有以下四种：乳液聚合法、悬浮聚合法、分散聚合法、种子溶胀法。乳液聚合只能制备粒径为0.1～0.7μm的颗粒且制备方法复杂，微球颗粒大小不一，分布不均匀。悬浮聚合制备的聚合物微球粒径则一般在100～1000μm之间，且是多分散性的。采用无皂或低皂乳液聚合法制成的单分散聚合物微球粒径接近1μm，但难于制备粒径大于1μm的聚合物微球。20世纪70年代发展起来的分散聚合法可制备粒径在1～100μm的单分散微球，制备方法比较复杂，而且需使用大量的有机溶剂(如乙醇)和稳定剂(聚乙烯吡咯烷酮等)，这样不仅影响聚合物的纯度，且给后处理带来困难。种子溶胀法的反应条件苛刻工艺繁琐。At present, there are mainly four ways to prepare polystyrene microspheres: emulsion polymerization, suspension polymerization, dispersion polymerization, and seed swelling method. Emulsion polymerization can only prepare particles with a particle size of 0.1-0.7 μm and the preparation method is complicated, and the microspheres have different sizes and uneven distribution. The particle size of polymer microspheres prepared by suspension polymerization is generally between 100 and 1000 μm, and they are polydisperse. The particle size of monodisperse polymer microspheres prepared by soap-free or low-soap emulsion polymerization is close to 1 μm, but it is difficult to prepare polymer microspheres with a particle size larger than 1 μm. The dispersion polymerization method developed in the 1970s can prepare monodisperse microspheres with a particle size of 1-100 μm. The preparation method is relatively complicated, and a large amount of organic solvents (such as ethanol) and stabilizers (polyvinylpyrrolidone, etc.) are required. This not only affects the purity of the polymer, but also brings difficulties to post-processing. The reaction conditions of the seed swelling method are harsh and the process is cumbersome.
有鉴于上述的缺陷，本设计人，积极加以研究创新，以期创设一种水溶性聚苯乙烯纳米微球的制备方法，使其更具有产业上的利用价值。In view of the above-mentioned defects, the designers actively researched and innovated in order to create a preparation method of water-soluble polystyrene nano-microspheres, so that it has more industrial utilization value.
发明内容Contents of the invention
本发明的目的是提供一种水溶性聚苯乙烯纳米微球的制备方法，本方法采用辐射一步法制备水溶性聚苯乙烯纳米微球，合成方法快速简单、成本低廉、产量大、合成的聚苯乙烯微球能很好的溶于水。The purpose of the present invention is to provide a method for preparing water-soluble polystyrene nano-microspheres. The method adopts a radiation one-step method to prepare water-soluble polystyrene nano-microspheres. Styrene microspheres are well soluble in water.
本发明提出的一种水溶性聚苯乙烯纳米微球的制备方法，包括以下步骤：A kind of preparation method of water-soluble polystyrene nano microsphere that the present invention proposes, comprises the following steps:
(1)将苯乙烯单体与去离子水混合，配制出A混合液；(1) mixing styrene monomer with deionized water to prepare a mixed solution of A;
(2)将A混合液置于辐照容器中密封，通入氮气，然后利用钴源或电子束进行辐照交联，获得产物，将产物冷冻干燥或真空干燥获得最终产品。(2) Put the mixed solution A in an irradiation container and seal it, blow nitrogen into it, and then use a cobalt source or an electron beam to irradiate and cross-link to obtain a product, and freeze-dry or vacuum-dry the product to obtain the final product.
进一步的，所述A混合液中，苯乙烯的体积百分数为1-90％。Further, in the mixed solution A, the volume percentage of styrene is 1-90%.
进一步的，辐射交联的剂量为10KGy-100KGy。Further, the dose of radiation crosslinking is 10KGy-100KGy.
借由上述方案，本发明至少具有以下优点：本方法采用辐射一步法制备水溶性聚苯乙烯纳米微球，原料为苯乙烯单体和去离子水，不掺杂其他试剂，获得水溶性聚苯乙烯纳米颗粒更加纯净；合成方法快速简单、成本低廉、产量大、合成的聚苯乙烯微球能很好的溶于水。By means of the above scheme, the present invention has at least the following advantages: the method adopts a radiation one-step method to prepare water-soluble polystyrene nano-microspheres, the raw materials are styrene monomer and deionized water, and no other reagents are mixed to obtain water-soluble polystyrene nanospheres. Ethylene nanoparticles are more pure; the synthesis method is fast and simple, the cost is low, the output is large, and the synthesized polystyrene microspheres can be well dissolved in water.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。The above description is only an overview of the technical solutions of the present invention. In order to understand the technical means of the present invention more clearly and implement them according to the contents of the description, the preferred embodiments of the present invention and accompanying drawings are described in detail below.
附图说明Description of drawings
图1是本发明实施例1中聚苯乙烯纳米微球的扫描电子显微镜图；Fig. 1 is the scanning electron micrograph of polystyrene nano microsphere in the embodiment of the present invention 1;
图2是本发明实施例1中聚苯乙烯纳米微球在另一标尺下的扫描电子显微镜图；Fig. 2 is the scanning electron micrograph of polystyrene nano-microspheres under another scale in the embodiment of the present invention 1;
图3是本发明实施例6中聚苯乙烯纳米微球的扫描电子显微镜图；Fig. 3 is the scanning electron micrograph of polystyrene nano microsphere in the embodiment of the present invention 6;
图4是本发明实施例6中聚苯乙烯纳米微球在另一标尺下的扫描电子显微镜图。Fig. 4 is a scanning electron microscope image of polystyrene nano-microspheres in Example 6 of the present invention under another scale.
具体实施方式detailed description
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。The specific implementation manners of the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
实施例1Example 1
取1mL的苯乙烯溶于99mL去离子水中，置于辐照瓶中，通入氮气。于钴源中辐照，辐照剂量为10KGy，得到1％聚苯乙烯纳米颗粒溶液，颗粒大小约500nm。Dissolve 1 mL of styrene in 99 mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in a cobalt source with a radiation dose of 10KGy to obtain a 1% polystyrene nanoparticle solution with a particle size of about 500nm.
实施例2Example 2
取1mL的苯乙烯溶于99mL去离子水中，置于辐照瓶中，通入氮气。于钴源中辐照，辐照剂量为100KGy，得到1％聚苯乙烯纳米颗粒溶液,颗粒大小约10nm。Dissolve 1 mL of styrene in 99 mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in a cobalt source with a radiation dose of 100KGy to obtain a 1% polystyrene nanoparticle solution with a particle size of about 10nm.
实施例3Example 3
取1mL苯乙烯溶于99mL的去离子水中，置于辐照瓶中，通入氮气。于钴源中辐照，辐照剂量为30KGy，得到1％聚苯乙烯纳米颗粒溶液,颗粒大小约20nm。Dissolve 1 mL of styrene in 99 mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in a cobalt source with a radiation dose of 30KGy to obtain a 1% polystyrene nanoparticle solution with a particle size of about 20nm.
实施例4Example 4
取90mL的苯乙烯溶于10mL的去离子水中，置于辐照瓶中，通入氮气。于钴源中辐照，辐照剂量为30KGy，得到50％聚苯乙烯纳米颗粒溶液,颗粒大小约20nm。Dissolve 90mL of styrene in 10mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in a cobalt source with a radiation dose of 30KGy to obtain a 50% polystyrene nanoparticle solution with a particle size of about 20nm.
实施例5Example 5
取50mL苯乙烯溶于50mL的去离子水中，置于辐照瓶中，通入氮气。于钴源中辐照，辐照剂量为30KGy，得到1％聚苯乙烯纳米颗粒溶液,颗粒大小约20nm。Dissolve 50mL of styrene in 50mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in a cobalt source with a radiation dose of 30KGy to obtain a 1% polystyrene nanoparticle solution with a particle size of about 20nm.
实施例6Example 6
取1mL的苯乙烯溶于99mL去离子水中，置于辐照瓶中，通入氮气。于电子束中辐照，辐照剂量为10KGy，得到1％聚苯乙烯纳米颗粒溶液，颗粒大小约300nm。Dissolve 1 mL of styrene in 99 mL of deionized water, place it in an irradiation bottle, and blow it with nitrogen. Irradiate in an electron beam with a radiation dose of 10KGy to obtain a 1% polystyrene nanoparticle solution with a particle size of about 300nm.
综上所述，本发明采用辐射一步法制备水溶性聚苯乙烯纳米微球，产物分布均匀一致，纳米颗粒大小均匀，而且成本低廉、产量大、合成的聚苯乙烯纳米微球能很好的溶于水；原料为苯乙烯单体和去离子水，反应物简单，不用掺杂其它试剂，获得的水溶性聚苯乙烯纳米颗粒更加纯净，无其他副产物，便于以后工业上的大量生产；而且苯乙烯单体反应前不需要进行前处理，简化了操作步骤，使整个工艺流程更加快速简单；通过调整苯乙烯单体的用量以及辐射交联的剂量，可以控制聚苯乙烯纳米颗粒的大小，满足不同生产需求。In summary, the present invention adopts the radiation one-step method to prepare water-soluble polystyrene nano-microspheres, the product distribution is uniform, the size of the nanoparticles is uniform, and the cost is low, the output is large, and the synthetic polystyrene nano-microspheres can be used very well. Soluble in water; the raw materials are styrene monomer and deionized water, the reactants are simple, without doping with other reagents, the obtained water-soluble polystyrene nanoparticles are more pure, without other by-products, which is convenient for mass production in the future; Moreover, no pretreatment is required before the reaction of styrene monomer, which simplifies the operation steps and makes the whole process faster and simpler; by adjusting the amount of styrene monomer and the dose of radiation crosslinking, the size of polystyrene nanoparticles can be controlled , to meet different production needs.
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. It should be pointed out that for those of ordinary skill in the art, some improvements can be made without departing from the technical principle of the present invention. and modifications, these improvements and modifications should also be considered as the protection scope of the present invention.
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| WO2008098339A1 (en) * | 2007-02-16 | 2008-08-21 | The Governing Council Of The University Of Toronto | Compressible photonic crystal |
| CN102010476B (en) * | 2010-11-02 | 2012-07-11 | 江南大学 | A method for preparing monodisperse polymer microspheres by ultraviolet light irradiation polymerization |
| CN102020811B (en) * | 2010-11-15 | 2013-03-27 | 北京师范大学 | Method for preparing polystyrene/conductive polymer composite hollow microspheres |
| CN102070829A (en) * | 2010-12-20 | 2011-05-25 | 北京化工大学 | Microsphere polypropylene beta nucleating agent and preparation method thereof |
| CN104530273A (en) * | 2014-09-19 | 2015-04-22 | 北京化工大学 | Preparation method of hydroxyl-terminated styrene resin |
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