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Preparation method of polyorganosiloxane hollow microsphere molecular box

A polyorganosiloxane and hollow microsphere technology, applied in the field of fine chemical industry, can solve the problems of limited stability and structural change, and achieve the effect of high biocompatibility and good aggregation and tolerance.

Inactive Publication Date: 2004-12-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitation of template particle size, it is difficult to prepare nano-ultrafine particles with a core-shell structure with a diameter of less than 100 nm, but the introduction of self-assembly and template methods makes it possible to prepare microsphere molecular boxes in the nanometer range
Experiments have shown that although the supramolecular structure formed by the self-assembly of amphiphilic polymers is one of the effective ways to prepare core-shell structures, it provides a structural template for the preparation of hollow microsphere molecular boxes at the nanometer level, However, since the supramolecular structure is a metastable structure formed through non-covalent interactions, its stability is limited, which can easily lead to structural changes.

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0011] (1) Preparation of the template core: Add the electrolyte quaternary ammonium salt type surfactant into the aqueous solution containing the basic catalyst, and stir to emulsify it. Slowly add dialkyldialkoxysilane dropwise at room temperature, continue to stir, and add trialkylalkoxysilane as an end-capping agent to deactivate the hydroxyl group at the end of polydialkylsiloxane, that is, to obtain a polydialkylsiloxane containing O / W Microemulsion Template Core of Linear Polydialkylsiloxane.

[0012] (2) Preparation of core-shell structure microsphere molecular box: Slowly add the mixture of organosilicon monomers containing T-type functional groups and D-type functional groups into the above-mentioned microemulsion, and stir for 8 to 12 hours. The trialkylalkoxysilane of the capping agent was capped twice again to prevent the remaining active silanol groups from condensation between microsphere molecular boxes. After the reaction, methanol was added to precipitate th...

Embodiment 1

[0021]In a 500 mL three-necked flask equipped with a mechanical stirrer, a reflux condenser, and a constant pressure dropping funnel, add 125 g of deionized water and 0.030 g of sodium hydroxide. After stirring and dissolving, add 3.0 g of surfactant isooctylbenzene polyethoxy dimethyl benzyl ammonium chloride (benzethonium chloride), stir to make it emulsified. At room temperature, 11.0 g of dimethyldimethoxysilane was slowly added dropwise from a constant pressure dropping funnel, stirring vigorously while adding, and the addition time was controlled at 1 hour. After the addition was complete, stirring was continued for 12 hours. Then 1.3 g of end-capping agent trimethylmethoxysilane was added to deactivate the polydimethylsiloxane terminal group capping. Mix 10.0 grams of methyltrimethoxysilane and 4.0 grams of dimethyldimethoxysilane, and slowly add the mixed solution dropwise to the above reaction solution from a constant pressure dropping funnel for 1 hour, and continue...

Embodiment 2

[0023] In a 500mL three-necked flask equipped with a mechanical stirrer, a reflux condenser, and a constant pressure dropping funnel, dissolve 0.050 grams of potassium bicarbonate in 125 grams of deionized water, and then add 3.0 grams of isooctylbenzene to the aqueous solution. Polyethoxy dimethyl benzyl ammonium chloride (benzethonium chloride), stirred to emulsify. At room temperature, 22.4 g of diphenyldimethoxysilane was slowly added dropwise from a constant pressure dropping funnel. Stir vigorously while adding dropwise, and the addition time is controlled at 1 hour. After the addition was complete, stirring was continued for 12 hours. Then 0.10 g of trimethylmethoxysilane was added to deactivate the polydiphenylsiloxane end group capping. 10.0 g of methyltrimethoxysilane and 8.2 g of diphenyldimethoxysilane were mixed, and the mixed solution was added dropwise to the above reaction solution, the dropping time was controlled at 1 hour, and the stirring reaction was con...

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Abstract

The present invention is the preparation process of hollow microspheric polyorganosilane molecular box, and features that on O / W type microemulsion polydialkyl siloxane template kernel, organosilicon monomer with D-type functional group and T-type functional group is added for condensation around the surface of the template kernel to form polyorganosilane microsphere in core-shell structure, and then solvent swelling dialysis method is adopted to eliminate the template kernel and to obtain hollow microspheric molecular box. The hollow microspheric polyorganosilane molecular box thus prepared has average diameter of 80-180 nm, good swelling and coating performance, and may be surface modified to reach required hydrophilic and lipophilic property. The hollow microspheric polyorganosilane molecular box has good biocompatibility, biodegradability and physiological inertia, and may be used widely.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing a polyorganosiloxane hollow microsphere molecular box. technical background [0002] In recent years, the research on self-assembled systems with core-shell structure is a very active field at home and abroad. With the deepening of research on polymer microspheres with core-shell structure, the research on hollow polymer microspheres has also attracted widespread attention. focus on. Supramolecules refer to metastable systems with specific structures and functions formed by non-covalent bonds between species, while molecular boxes refer to supramolecular structures based on the structure of supramolecules, through polycondensation, to co- Therefore, the stability of non-covalent interactions of supramolecular structures is limited, which can easily lead to structural changes. In addition to maintaining the original characte...

Claims

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Application Information

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IPC IPC(8): C08G77/38
Inventor 陈平王惠钢郑小明
Owner ZHEJIANG UNIV
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