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A kind of preparation method of cyclodextrin microsphere

A cyclodextrin and microsphere technology, used in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc. The post-processing is cumbersome and other problems, to achieve the effect of good monodispersity, high recycling rate, and convenient separation and recovery

Active Publication Date: 2022-01-18
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of method has cumbersome post-processing: it is necessary to add a demulsifier to demulsify the emulsifier to expose the microspheres; the oil phase obtained after demulsification contains various impurities such as emulsifiers, resulting in a low reuse rate of the oil phase; the obtained The particle size uniformity of the microspheres still needs to be improved

Method used

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  • A kind of preparation method of cyclodextrin microsphere
  • A kind of preparation method of cyclodextrin microsphere
  • A kind of preparation method of cyclodextrin microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Dissolve 2g of β-cyclodextrin in 4mL of NaOH solution with a mass fraction of 20%, alkalinize with stirring at 40°C for 0.5h, and then add 2.4g of epichlorohydrin for pre-crosslinking for 2.5h. to stir. After the reaction, a liquid and viscous pre-crosslinked product is obtained.

[0033] (2) Mix the pre-crosslinked product with 25# transformer oil at a volume ratio of 1:2, and stir at 100r / min at 40°C until the pre-crosslinked product exists completely in the form of microspheres.

[0034] (3) The product after the reaction is left to stand for about 10min, and after the microsphere particles in the oil phase are completely precipitated, the upper oil phase is sucked out and recovered with a straw, and the microsphere particles are rinsed with distilled water and then soaked in absolute ethanol for 24h. Remove the residual oil phase inside the microsphere particles.

[0035] (4) Dry the microsphere particles in a vacuum oven at 50°C to constant weight to obtain β...

Embodiment 2

[0037] (1) Dissolve 2g of β-cyclodextrin in 4mL of NaOH solution with a mass fraction of 20%, alkalinize with stirring at 40°C for 0.5h, then add 2.4g of glutaraldehyde for pre-crosslinking for 1h, supplemented with 100~ Stir at 300r / min. After the reaction, a liquid and viscous pre-crosslinked product is obtained.

[0038] (2) Mix the pre-crosslinked product and lubricating oil at a volume ratio of 1:3, and stir at 300r / min at 40°C until the pre-crosslinked product exists completely in the form of microspheres.

[0039] (3) The product after the reaction is left to stand for about 10min, and after the microsphere particles in the oil phase are completely precipitated, the upper oil phase is sucked out and recovered with a straw, and the microsphere particles are rinsed with distilled water and then soaked in absolute ethanol for 24h. Remove the residual oil phase inside the microsphere particles.

[0040] (4) Dry the microsphere particles in a vacuum oven at 50°C to constant...

Embodiment 3～5

[0042] Using almost the same treatment as in Example 1, only the stirring rate in the pre-crosslinked product / oil phase reaction process (step (2)) is adjusted: the stirring rate is adjusted to 300, 700 and 1000r / min respectively, as an implementation The processing of examples 3 to 5 (the stirring rate corresponding to embodiment 3 is 300r / min, the corresponding 700r / min of embodiment 4, and the corresponding 1000r / min of embodiment 5).

[0043] control treatment

[0044] On the basis of the treatment in Example 3, the simple oil phase used in step (2) was changed to the oil phase added with an emulsifier (equivalent to the conventional inverse emulsion polymerization method), as control treatment 1. Wherein, the emulsifier is a mixture of Span-80 and Tween-20, m(Span-80):m(Tween-20)=3:1, and the mass ratio of the emulsifier to the oil phase is 1:30. Control treatment 2 of Example 4 and control treatment 3 of Example 5 were set in the same manner.

[0045] The microspheres ...

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Abstract

The invention discloses a preparation method of cyclodextrin microspheres: the cyclodextrin is alkalized and then added with a cross-linking agent for pre-cross-linking for a period of time, then the pre-cross-linked product and the oil phase are mixed in a certain proportion, and the reaction is stirred until The pre-crosslinked product becomes microsphere particles; after standing until the microsphere particles in the oil phase are completely precipitated, the upper oil phase is sucked out and recovered, and the obtained microsphere particles are rinsed with distilled water and transferred to absolute ethanol for soaking and washing. Then dry to constant weight to obtain β-cyclodextrin microspheres. Compared with the conventional inverse emulsion polymerization method, the present invention has the following advantages: the preparation steps are simple, the reagents required are few, the oil phase does not need to add emulsifier, and oil-water separation can be directly carried out after the reaction; the subsequent treatment of the obtained microspheres is simple; the oil phase is separated The recovery is more convenient and the recycling rate is higher; the particle size distribution of the obtained microspheres is more in line with the normal distribution and the particle size distribution is more concentrated; the particle size of the microspheres can be easily and effectively controlled during the preparation process, and microspheres with different particle sizes can be obtained. ball.

Description

Technical field: [0001] The invention relates to the field of polymer microspheres, in particular to a preparation method of cyclodextrin microspheres. Background technique: [0002] Cyclodextrin has a special structure with a hydrophilic exterior and a hydrophobic interior. It is an excellent structural unit. Its polymers have been widely used in various fields: catalysis, chiral separation, drug loading and slow release, and adsorption of environmental pollutants. Wait. Cyclodextrin molecules can still retain cavities and hydroxyl groups in the polymer, which provides the possibility for cyclodextrin polymers to include organic and inorganic guest molecules, and people can design and develop different properties and functions according to actual needs. Cyclodextrin polymer material. [0003] Polymer microspheres are a kind of functional polymer materials, which have a variety of excellent properties: uniformity, regularity of structure, large specific surface area and ea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L5/16B01J20/24B01J20/28B01J20/30C02F1/28
CPCC08J3/24B01J20/24B01J20/28021C02F1/286C08J2305/16
Inventor 刘泽华郑进智池凯石爽
Owner TIANJIN UNIV OF SCI & TECH
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