阅读说明：本技术 一种单分散胶体乳液的制备方法 (Preparation method of monodisperse colloid emulsion ) 是由 陈苏 于晓晴 于 2020-12-31 设计创作，主要内容包括：本发明公开了一种单分散胶体乳液的制备方法,配制质量浓度为5-15％的单分散胶体粒子水分散液作为反应底液,加入质量浓度为0.5-1.0％的基团活化剂水溶液进行搅拌活化；活化完成后,滴加质量浓度为0.5-1.5％的功能性粒子水溶液进行负载；将体系搅拌反应,离心除去未负载的功能性粒子,即得到具有功能性铠甲的单分散胶体乳液。本发明制备的具有功能性铠甲的单分散胶体乳液的单分散性良好,绿色环保,单分散指数低于5％,操作手段简单高效,经济效益高。制备的具有功能性铠甲的单分散胶体乳液是组装高质量光子晶体材料的一种新型理想构筑单元。(The invention discloses a preparation method of monodisperse colloidal emulsion, which comprises the steps of preparing 5-15% monodisperse colloidal particle water dispersion as reaction base solution, adding 0.5-1.0% group activator aqueous solution, stirring and activating; after activation, dropwise adding a functional particle aqueous solution with the mass concentration of 0.5-1.5% for loading; and (3) stirring the system for reaction, and centrifuging to remove the unloaded functional particles to obtain the monodisperse colloidal emulsion with the functional armor. The monodisperse colloidal emulsion with the functional armor prepared by the invention has the advantages of good monodispersity, environmental protection, monodispersity index lower than 5%, simple and efficient operation means and high economic benefit. The prepared monodisperse colloidal emulsion with functional armor is a novel ideal building unit for assembling high-quality photonic crystal materials.)

1. A preparation method of monodisperse colloid emulsion comprises the following specific steps:

a. preparing 5-15% of monodisperse colloidal particle water dispersion as reaction base solution, adding 0.5-1.0% of group activator aqueous solution, stirring and activating;

b. after activation, dropwise adding a functional particle aqueous solution with the mass concentration of 0.5-1.5% for loading;

c. stirring the system for reaction, and centrifuging to obtain the monodisperse colloidal emulsion with the functional armor;

wherein the mass percent of the reaction base solution in the whole reaction system is 45-55%, the mass percent of the activating agent aqueous solution in the whole reaction system is 25-40%, and the mass percent of the functional particle aqueous solution in the whole reaction system is 15-28%.

2. The method according to claim 1, wherein the monodisperse colloidal particles in step a are silica monodisperse colloidal particles, polymethyl methacrylate monodisperse colloidal particles having carboxyl groups, or polystyrene monodisperse colloidal particles having carboxyl groups.

3. The method according to claim 1, wherein the radical activator in step a is one or two of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 4-dimethylaminopyridine and N-hydroxysuccinimide.

4. The method according to claim 1, wherein the stirring activation time in step a is 40-60 min.

5. The method according to claim 1, wherein the functional particles in step b are one of hematoxylin, buddlein and anthocyanin.

6. The method as claimed in claim 1, wherein the centrifugation speed in step c is 14000-16000rad/min for 15-20 min.

7. The preparation method according to claim 1, wherein the reaction temperature is constant at 20-30 ℃ and the reaction time is 8-10 h; the mechanical stirring speed is constant at 200-250 rpm.

8. The method according to claim 1, wherein the monodisperse colloid emulsion is prepared to have a monodispersity index of 2.0 to 3.5%; the particle size range is 220-310 nm.

Technical Field

The invention relates to a preparation method of a monodisperse colloidal emulsion, in particular to a preparation method of a monodisperse colloidal emulsion with functional armor, which can be used as a novel ideal construction unit for assembling high-quality photonic crystal materials.

Background

Photonic crystals having unique photonic band gaps have received much attention, and photonic crystals can exhibit bright structural colors by reflecting visible light of specific wavelengths. The method for constructing the photonic crystal by utilizing the ordered self-assembly of the monodisperse colloidal particles is widely applied to the development of various photonic crystal materials by people due to the characteristics of universality, controllability, economy and high efficiency. The structural color saturation of the colloidal photonic crystal is greatly reduced due to the existence of defects and coherent light scattering caused by particle stacking in the assembly process of the colloidal particles and the influence of ambient background light. Many attempts have been made to develop high brightness, high saturation structure chromophorous photonic crystals. For example, ZHENGDONG Cheng et al enhances the structural color visibility of the colloidal photonic crystal by co-assembling the thioglycerol-modified graphene quantum dots and the polystyrene nanoparticles; ming Xiao et al propose low refractive index silica as the core and high refractive index synthetic melanin as the shell, and core-shell colloidal particles as the building units of photonic crystals to achieve high brightness of structural color. These methods have been successful in achieving high saturation and high brightness of photonic crystal structural colors. But the method needs multi-step operation, has more limitation conditions, and is time-consuming and labor-consuming.

Disclosure of Invention

The invention aims to provide a preparation method of monodisperse colloidal emulsion, and colloidal particles prepared by the method have good monodispersity, uniform appearance and adjustable particle size. Can be used as a novel ideal construction unit for assembling high-quality photonic crystal materials. And the whole preparation process has simple equipment and convenient and fast operation, and is an efficient method for the functionalized monodisperse colloid emulsion. The colloidal emulsion is environment-friendly and green, and can absorb background ambient light in a specific wavelength range. And coherent light scattering generated in the assembly process of the colloidal particles is inhibited, so that the color saturation and brightness of the photonic crystal structure are improved.

The invention is mainly realized by the following technical scheme: a preparation method of monodisperse colloid emulsion comprises the following specific steps:

a. preparing 5-15% of monodisperse colloidal particle water dispersion as reaction base solution, adding 0.5-1.0% of group activator aqueous solution, stirring and activating;

b. after activation, dropwise adding a functional particle aqueous solution with the mass concentration of 0.5-1.5% for loading;

c. stirring the system for reaction, and centrifuging to remove the unloaded functional particles to obtain the monodisperse colloidal emulsion with the functional armor;

wherein the mass percent of the reaction base solution in the whole reaction system is 45-55%, the mass percent of the activating agent aqueous solution in the whole reaction system is 25-40%, and the mass percent of the functional particle aqueous solution in the whole reaction system is 15-28%.

Preferably, the monodisperse colloidal particles in step a are silica monodisperse colloidal particles, polymethyl methacrylate monodisperse colloidal particles having carboxyl groups, or polystyrene monodisperse colloidal particles having carboxyl groups.

Preferably, the radical activator in step a is one or two of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 4-dimethylaminopyridine or N-hydroxysuccinimide.

Preferably, the stirring activation time in the step a is 40-60 min;

preferably, the functional particles in step b are one of hematoxylin, buddlein or anthocyanin.

Preferably, the centrifugation speed in the step c is 14000-16000rad/min and the time is 15-20 min.

Preferably, in the whole reaction process, the reaction temperature is kept constant at 20-30 ℃, and the reaction time is 8-10 h; the mechanical stirring speed is constant at 200-250 rpm;

preferably, the monodispersion index of the prepared monodisperse colloid emulsion is 2.0-3.5%; the particle size range is 220-310 nm.

The synthesized monodisperse colloid emulsion has adjustable particle size, good monodispersity, environmental protection, safety, simple and efficient operation means and high economic benefit. Is a novel ideal building unit for assembling high-quality photonic crystal materials.

Biological functional particles such as hematoxylin, buddlein and anthocyanin, and the like are green, safe and wide in source. The inherent nature of these biofunctional particles enables them to form a variety of non-covalent interactions, including hydrogen bonding, electrostatic interactions and aromatic stacking. Therefore, they were selected as functional particles to prepare monodisperse colloidal emulsions with functional armor by a simple one-step in situ loading process. The functionalized monodisperse colloid particles can be obtained by simple one-step in-situ loading, a foundation is laid for the development of functionalized colloid photonic crystal materials, and the in-situ loading method is used as an environment-friendly and green method for preparing monodisperse colloid emulsion, so that the product cost can be reduced and the post-treatment process can be reduced. The monodisperse polymer colloid emulsion has wide application prospect in the fields of coating, papermaking, display, anti-counterfeiting and the like. Therefore, it is particularly important to prepare monodisperse colloidal emulsions with functional armor using a one-step in situ loading process.

Has the advantages that:

1. the monodisperse colloid emulsion with the functional armor prepared by the invention has good monodispersity, uniform appearance, adjustable particle size and environmental protection;

2. the preparation method of the monodisperse colloidal emulsion with the functional armor has the advantages that the whole preparation process is simple in equipment, convenient and fast to operate, economical and efficient;

3. the monodisperse colloidal emulsion with the functional armor prepared by the invention can be used as a novel ideal construction unit for assembling high-quality photonic crystal materials, and can inhibit coherent light scattering generated in the assembly process of colloidal particles so as to improve the saturation and brightness of the structural color of the photonic crystal.

Drawings

FIG. 1 is an SEM image of a monodisperse colloidal emulsion with functional armor made according to example 1;

FIG. 2 is a particle size distribution plot of a monodisperse colloidal emulsion with functional armor prepared in example 1;

FIG. 3 is a plot of the reflectance spectrum of a monodisperse colloidal emulsion with functional armor made according to example 1.

Detailed Description

The present invention is illustrated below by means of specific examples, but the present invention is not limited to the following examples, which are only intended to better understand the present invention and not to limit the scope of protection of the present invention.

Example 1

Preparing 4g of 10 wt% silica monodisperse colloidal particle water dispersion as a reaction base solution, adding 2g of 0.5 wt% 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride aqueous solution, and performing constant mechanical stirring at 200rpm at room temperature for activation for 40 min; then adding 2g of 0.5 wt% hematoxylin water solution, continuously stirring and loading for 8h at 30 ℃, centrifuging for 15min at 14000rad/min to remove the unloaded hematoxylin particles, and obtaining the monodisperse colloid emulsion with the functional armor. From the SEM image of FIG. 1, it can be seen that the colloidal particles are uniform in morphology and exhibit regular and ordered close arrangement of regular hexagons. The particle size distribution chart of FIG. 2 shows that the monodisperse colloidal emulsion prepared has an average particle size of 227nm and a PDI value of 2.0%. The reflectance spectrum of fig. 3 shows that the monodisperse colloidal emulsion of functional armor assembled photonic crystals with high peak intensity, low background and narrow half-peak width.

Example 2

Preparing 7g of 15 wt% of polystyrene monodisperse colloidal particle aqueous dispersion with carboxyl as reaction base solution, adding 2g of 0.8 wt% of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride aqueous solution and 2g of 0.8 wt% of 4-dimethylaminopyridine aqueous solution, and performing constant mechanical stirring at 230rpm at room temperature for activation for 50 min; then adding 2g of 1.0 wt% of buddlein aqueous solution, continuously stirring and loading for 9h at 25 ℃, centrifuging for 18min at 15000rad/min to remove the non-loaded buddlein particles, and obtaining the monodisperse colloid emulsion with the functional armor. The average particle diameter of the prepared monodisperse colloid emulsion is 287nm, and the PDI value of the emulsion is 3.1%. The colloidal particles have uniform appearance and are regularly and orderly arranged in a regular hexagon. The assembled photonic crystal has high reflection peak intensity, low background value and narrow half-peak width.

Example 3

Preparing 5g of 5 wt% of aqueous dispersion of monodisperse colloidal particles of polymethyl methacrylate with carboxyl as reaction base solution, adding 2g of aqueous solution of 1.0 wt% of 4-dimethylaminopyridine and 2g of aqueous solution of 0.8 wt% of N-hydroxysuccinimide, and performing constant mechanical stirring at 240rpm at room temperature for activation for 60 min; then adding 2g of 1.5 wt% anthocyanin aqueous solution, continuously stirring and loading for 10h at 20 ℃, centrifuging for 20min at 16000rad/min to remove unloaded anthocyanin particles, and obtaining the monodisperse colloid emulsion with the functional armor. The average particle size of the prepared monodisperse colloid emulsion was 307nm, and the PDI value of the emulsion was 2.7%. The colloidal particles have uniform appearance and are regularly and orderly arranged in a regular hexagon. The assembled photonic crystal has high reflection peak intensity, low background value and narrow half-peak width.