张俊丰1,
黄妍1,
田凯勋1,
赵令葵1
1.湘潭大学环境与资源学院, 湘潭 411105
基金项目: 湖南省教育厅创新平台项目资助（16K087）
湖南省重点研发计划项目（2018SK2018）
Preparation and application of microcapsule catalytic materials with precisely regulated particle size
FU Hui1,,ZHANG Junfeng1,
HUANG Yan1,
TIAN Kaixun1,
ZHAO Lingkui1
1.College of Environment and Resources, Xiangtan University, Xiangtan 411105, China
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摘要:提出基于核材与壳材粒径双调控的微胶囊催化材料制备新思路，通过旋风分级和气力乳化聚合工艺优化，最终实现微胶囊的粒径调控。重点考察了气力乳化工艺参数和核材粒径、核壳材料质量比等对微胶囊平均粒径、粒径分布和包覆率的影响。实验结果表明：当气力乳化的气体流速为1.12 m·s-1时，壳材液滴的融合和乳胶粒的粘并现象均较少，聚合体系可较稳定地保持均质化壳材液滴的尺寸；在保证高包覆率的条件下，核材粒径影响着微胶囊的平均粒径，核材粒径为15.4 μm时，制备出的微胶囊平均粒径最小；核壳材料质量比对微胶囊粒径的影响明显，其为1:3.5时，微胶囊材料平均粒径为180 μm；亲水亲油平衡值（HLB）对粒径调控能力有限，平均粒径最小时微胶囊包覆率最大。通过对乳化聚合工艺和配方的综合调节，可制得一系列粒径可调范围大，粒径均一，包覆率高的微胶囊材料，应用于烟气脱硝，温度600 ℃条件下，NOx转化率可达92%。
关键词: 粒径/
双调控/
微胶囊/
氮氧化物
Abstract:A new idea of microcapsule catalytic material preparation based on double-regulation of the particle and shell material size was proposed. The cyclone grading and pneumatic emulsification polymerization process were optimized to achieve the particle size regulation of microcapsules. The effects of pneumatic emulsification process parameters, nuclear material particle size and core-shell material mass ratio on the average particle size, particle size distribution and coating ratio of microcapsules were investigated. The results showed that when the gas emulsified gas flow rate was 1.12 m·s-1, the fusion of shell droplets and the adhesion of latex particles were less, and the polymerization system could stably homogenize the shell droplets. Under the condition of high coverage, the average particle size of the microcapsules was depended on the size of the core material. The average particle size of the prepared microcapsules could reach the smallest value at the core material particle size of 15.4 μm. The core-shell material mass ratio had an obvious effect on the particle size of the microcapsules and the average particle size of the microcapsule material was 180 μm at the mass-ratio of 1:3.5. Hydrophilic-lipophilic balance (HLB) presented a limited regulation on particle size, and the microcapsule coating rate was the largest when the average particle size was the smallest. Through the comprehensive adjustment of the emulsion polymerization process and formulation, a series of microcapsule materials with a wide range of adjustable particle size, uniform particle size, and high coating rate could be obtained, which was used in the denitrification experiment and could get a 92% NOx conversion at a temperature of 600 ℃.
Key words:particle size/
double regulation/
microcapsules/
nitrogen oxides.
| [1] | 林书乐, 王坤. 微胶囊技术新进展[J]. 高分子材料科学与工程, 2012, 28(5):179-182 |
| [2] | LIU H.Preparation of phospholipid microcapsule by spray drying[J].Drying Technology, 2007, 25(4):695-702 |
| [3] | 李小芝, 张俊丰, 黄妍. 活性粉末脱硝剂制备及其催化还原NOx性能[J]. 环境工程学报, 2017, 11(8):4641-4646 10.12030/j.cjee.201701022 |
| [4] | CERDEIRA A M, GOUVEIA L F, GOUCHA P, et al.Drug particle size influence on enteric beads produced by a droplet extrusion/precipitation method[J].Journal of Microencapsulation, 2000, 17(6):733-741 10.1080/02652040050161729 |
| [5] | 林四发. 脂溶性高锰酸钾包覆颗粒的制备及去除TCE的研究[D]. 福州:福州大学, 2010 |
| [6] | KANG N, HUA I, RAO P S C.Production and characterization of encapsulated potassium permanganate for sustained release as an in situ oxidant[J].Industrial & Engineering Chemistry Research, 2004, 43(17):5187-5193 |
| [7] | DONG S S, WANG J, WANG Y L, et al .Preparation and releasing characteristics of controlled release potassium permanganate[J].Materials Science Forum, 2013, 744:782-788 10.4028/www.scientific.net/MSF.743-744.782 |
| [8] | YUAN B, CHEN Y, FU M L.Degradation efficiencies and mechanisms of trichloroethylene (TCE) by controlled-release permanganate (CRP) oxidation[J].Chemical Engineering Journal, 2012, 192(2):276-283 10.1016/j.cej.2012.03.049 |
| [9] | 李小芝. 活性粉末脱硝剂制备及其脱除NOx实验研究[D]. 湘潭: 湘潭大学, 2017 |
| [10] | ESQUISABEL A, HERNANDEZ R M, IGARTUA M, et al.Effect of lecithins on BCG-alginate-PLL microcapsule particle size and stability upon storage[J].Journal of Microencapsulation, 2000, 17(3):363-372 10.1080/026520400288328 |
| [11] | PEREVYAZK I, VOLLRATH A, HORING S, et al.Characterization of poly(methyl methacrylate) nanoparticles prepared by nanoprecipitation using analytical ultracentrifugation, dynamic light scattering, and scanning electron microscopy[J].Journal of Polymer Science Part A: Polymer Chemistry, 2010, 48(18):3924-3931 10.1002/pola.24157 |
| [12] | FENG J G, YANG G T, ZHANG S W, et al.Fabrication and characterization of β-cypermethrin-loaded PLA microcapsules prepared by emulsion-solvent evaporation: Loading and release properties[J].Environmental Science & Pollution Research International, 2018, 25(4):1-11 |
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| [14] | 戚栋明, 陈智杰, 赵晓丽, 等. 微悬浮法制备有机颜料微胶囊中的粒径调控[J]. 化工学报, 2013, 64(3):1118-1123 |
| [15] | 王辉, 张俊峰, 白云星,等.NiO@SiO2核壳催化剂在浆态床中低温甲烷化研究[J]. 燃料化学学报, 2016, 44(5):548-556 |
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粒径精确调控的微胶囊催化材料制备及应用
符辉1,,张俊丰1,
黄妍1,
田凯勋1,
赵令葵1
1.湘潭大学环境与资源学院, 湘潭 411105
基金项目: 湖南省教育厅创新平台项目资助（16K087） 湖南省重点研发计划项目（2018SK2018）
关键词: 粒径/
双调控/
微胶囊/
氮氧化物
摘要:提出基于核材与壳材粒径双调控的微胶囊催化材料制备新思路，通过旋风分级和气力乳化聚合工艺优化，最终实现微胶囊的粒径调控。重点考察了气力乳化工艺参数和核材粒径、核壳材料质量比等对微胶囊平均粒径、粒径分布和包覆率的影响。实验结果表明：当气力乳化的气体流速为1.12 m·s-1时，壳材液滴的融合和乳胶粒的粘并现象均较少，聚合体系可较稳定地保持均质化壳材液滴的尺寸；在保证高包覆率的条件下，核材粒径影响着微胶囊的平均粒径，核材粒径为15.4 μm时，制备出的微胶囊平均粒径最小；核壳材料质量比对微胶囊粒径的影响明显，其为1:3.5时，微胶囊材料平均粒径为180 μm；亲水亲油平衡值（HLB）对粒径调控能力有限，平均粒径最小时微胶囊包覆率最大。通过对乳化聚合工艺和配方的综合调节，可制得一系列粒径可调范围大，粒径均一，包覆率高的微胶囊材料，应用于烟气脱硝，温度600 ℃条件下，NOx转化率可达92%。
English Abstract
Preparation and application of microcapsule catalytic materials with precisely regulated particle size
FU Hui1,,ZHANG Junfeng1,
HUANG Yan1,
TIAN Kaixun1,
ZHAO Lingkui1
1.College of Environment and Resources, Xiangtan University, Xiangtan 411105, China
Keywords: particle size/
double regulation/
microcapsules/
nitrogen oxides
Abstract:A new idea of microcapsule catalytic material preparation based on double-regulation of the particle and shell material size was proposed. The cyclone grading and pneumatic emulsification polymerization process were optimized to achieve the particle size regulation of microcapsules. The effects of pneumatic emulsification process parameters, nuclear material particle size and core-shell material mass ratio on the average particle size, particle size distribution and coating ratio of microcapsules were investigated. The results showed that when the gas emulsified gas flow rate was 1.12 m·s-1, the fusion of shell droplets and the adhesion of latex particles were less, and the polymerization system could stably homogenize the shell droplets. Under the condition of high coverage, the average particle size of the microcapsules was depended on the size of the core material. The average particle size of the prepared microcapsules could reach the smallest value at the core material particle size of 15.4 μm. The core-shell material mass ratio had an obvious effect on the particle size of the microcapsules and the average particle size of the microcapsule material was 180 μm at the mass-ratio of 1:3.5. Hydrophilic-lipophilic balance (HLB) presented a limited regulation on particle size, and the microcapsule coating rate was the largest when the average particle size was the smallest. Through the comprehensive adjustment of the emulsion polymerization process and formulation, a series of microcapsule materials with a wide range of adjustable particle size, uniform particle size, and high coating rate could be obtained, which was used in the denitrification experiment and could get a 92% NOx conversion at a temperature of 600 ℃.
