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Preparation method of pH and temperature responsive double-shell hollow microspheres

A hollow microsphere and temperature-responsive technology, which is applied to the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems that the preparation technology needs to be improved, and achieve the advantages of simple and fast preparation method, low density and high luminous efficiency Effect

Active Publication Date: 2019-11-05
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the continuous development of hollow microspheres with environmental response and fluorescent properties has greatly promoted the progress in the field of biomedicine, but its preparation technology needs to be improved

Method used

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  • Preparation method of pH and temperature responsive double-shell hollow microspheres
  • Preparation method of pH and temperature responsive double-shell hollow microspheres
  • Preparation method of pH and temperature responsive double-shell hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Take 3.8mL of silane coupling agent vinyltriethoxysilane (KH-151) and 26.2mL of water, add it into a 100mL single-necked flask, and stir magnetically at room temperature until the mixture is uniform. Adjust the pH value of the solution system between 3 and 4 with dilute hydrochloric acid, and continue stirring for 1 hour to hydrolyze the solution under acidic conditions, and the solution turns from light white to transparent. Then use dilute ammonia solution to quickly adjust the pH value of the solution system to between 10 and 11, stop stirring, and let it stand for 15 hours. The product is separated, centrifuged with water and ethanol, washed ultrasonically for 3 to 5 times, and vacuum-dried at 50° C. to obtain polyvinylsiloxane (PVSI) microspheres.

[0050] figure 1 In the infrared spectrum of PVSI microspheres, 3433cm -1 is the Si-OH stretching vibration peak at 2933cm -1 Where is silicon vinyl (Si-CH=CH 2 ) in the Si-C bond absorption peak, 1544cm -1 where Si...

Embodiment 2

[0053] Add 0.2g of PVSI microspheres prepared in Example 1 to 40mL of acetonitrile, ultrasonically disperse for 10min, transfer to a 100mL two-necked flask, add 0.3g of methacrylic acid (MAA), 0.2g of crosslinking agent N,N'-methylene Bisacrylamide (MBA), 0.1g initiator azobisisobutyronitrile (AIBN), heating to reflux for polymerization reaction, distilling 20mL of acetonitrile within 1.5 to 2h to end the reaction. After centrifugation with acetonitrile and ethanol, ultrasonic washing, and vacuum drying at 50°C, cross-linked polysiloxane@polymethacrylic acid (PVSI@PMAA) core-shell microspheres were obtained.

[0054] image 3 The infrared spectra of the prepared PVSI@PMAA core-shell microspheres are given. In the picture, 3424cm -1 is the Si-OH stretching vibration peak, 1600cm -1 where Si-CH=CH 2 Stretching vibration absorption peak, 1709cm -1 is the C=O stretching vibration peak of carboxylic acid, 1134, 1032cm -1 The broad peak is the characteristic absorption peak of...

Embodiment 3

[0057] Add 0.2 g of the PVSI@PMAA core-shell microspheres prepared in Example 2 above and 2.4 mL of ammonia water into a three-necked flask filled with 20 mL of water and 160 mL of absolute ethanol, and, under vigorous stirring at room temperature, dissolve 0.8 mL of ethyl orthosilicate within 1 h. The ester (TEOS) was slowly added dropwise into the flask, and the stirring reaction was continued for 6h. Then 0.2 mL of vinyltriethoxysilane (KH-151) was slowly added into the solution, and the reaction was terminated after 18 hours of reaction. The product was centrifuged and washed with ethanol and water in sequence to prepare a cross-linked polysiloxane@polymethacrylic acid@silicon dioxide (PVSI@PMAA@SiO2) with double bonds on the surface. 2 -CH=CH 2 ) three-layer composite microspheres.

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Abstract

The invention discloses a preparation method of pH and temperature responsive double-shell hollow microspheres, and the preparation method comprises the following steps: preparing PVSI microspheres byvinyl triethoxysilane; crosslinking methacrylic acid on the surface of the PVSI microspheres to prepare PVSI @ PMAA core-shell microspheres; polycondensing the vinyl triethoxysilane on the surface ofthe PVSI @ PMAA core-shell microspheres to prepare PVSI @ PMAA @ SiO2-CH=CH2 three-layer composite microspheres; crosslinking poly N-isopropylacrylamide to prepare PVSI@PMAA@SiO2@PNIPAM four-layer composite microspheres, crosslinking an allyl fluorescent dye at the same time, and finally preparing air@PMAA@air@PNIPAM double-shell hollow microspheres by HF corrosion. The double-shell hollow microsphere has good monodispersity and simultaneously has pH responsiveness and temperature responsiveness.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic-organic fluorescent microspheres, and relates to a method for preparing hollow microspheres, in particular to a method for preparing hollow polymer fluorescent microspheres with pH and temperature responsiveness. Background technique [0002] Hollow microspheres not only have a special structure and morphology, but also have a large specific surface area, good thermal insulation, and low density. They are widely used in biomedicine, drug controlled release, catalysis, and thermal insulation coatings. Such as SiO 2 Hollow microspheres are loaded with anticancer drug doxorubicin hydrochloride, and the release of doxorubicin hydrochloride is controlled by controlling the temperature and pH value (Macromolecules, 2008,41, 9487-9490.); Precious metals Ag, Au, etc. are loaded on hollow microspheres , can serve as an important catalyst. [0003] A variety of physical and chemical metho...

Claims

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Application Information

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IPC IPC(8): C08F285/00C08F230/08C08F283/12C08F220/06C08F226/06C08G77/20B01J13/14C09K11/06
CPCB01J13/14C08F283/124C08F285/00C08G77/20C09K11/06C09K2211/145C09K2211/1466C08F220/06C08F226/06C08F230/08
Inventor 刘清浩郭金春刘红彦胡志勇
Owner ZHONGBEI UNIV
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