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Preparation of silicon dioxide microsphere with nonionic/anionic-combined-type surfactant as soft template

A surfactant and silica technology, which is applied in the preparation of non-ionic/anion-bound surfactants as soft templates and the preparation of silica hybrid microspheres, can solve the problem of small pore size and wall thickness of materials, Limit the application of microspheres, etc., to achieve the effects of increased solubility, improved antistatic, and uniform space size

Inactive Publication Date: 2016-08-31
广州赫尔普化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used block copolymers include polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (PEO-PPO-PEO), etc., but due to the limitation of its molecular weight, the obtained material pore size and wall thickness are relatively small, limiting the application of the resulting microspheres

Method used

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  • Preparation of silicon dioxide microsphere with nonionic/anionic-combined-type surfactant as soft template
  • Preparation of silicon dioxide microsphere with nonionic/anionic-combined-type surfactant as soft template
  • Preparation of silicon dioxide microsphere with nonionic/anionic-combined-type surfactant as soft template

Examples

Experimental program
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Effect test

Embodiment 1

[0050] 1. Synthesis of star-shaped hybrid arm polymers

[0051] (1) Synthesis of polymethyl methacrylate (PMMA): 6.25 g of methyl methacrylate, 0.375 g of RAFT reagent, 0.0125 g of AIBN, and 12.5 mL of toluene were charged into a flask. Perform freeze degassing several times. Polymerization was carried out at 60°C for 4 hours. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0052] (2) Synthesis of poly(methoxypolyethylene glycol acrylate) (P(PEGMEA)): 12.5g methoxypolyethylene glycol acrylate, 0.375g RAFT reagent, 0.0125gAIBN, 12.5mL toluene were loaded into a flask . Perform freeze degassing several times. Polymerization was carried out at 60°C for 1 hour. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0053] (3) Synthesis of poly(methyl methacrylate block styrene) (P(MMA-b-St)): 5 g of polymethyl ...

Embodiment 2

[0066] 1. Synthesis of star-shaped hybrid arm polymers

[0067] (1) Synthesis of polymethyl methacrylate (PMMA): 12.5 g of methyl methacrylate, 0.455 g of RAFT reagent, 0.0205 g of AIBN, and 12.5 mL of toluene were charged into a flask. Perform freeze degassing several times. Polymerization was carried out at 70°C for 4 hours. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0068] (2) Synthesis of poly(methoxypolyethylene glycol acrylate) (P(PEGMEA)): 15 g of methoxypolyethylene glycol acrylate, 0.0455 g of RAFT reagent, 0.0205 g of AIBN, and 12.5 mL of toluene were charged into a flask. Perform freeze degassing several times. Polymerization was carried out at 70°C for 1 hour. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0069] (3) Synthesis of poly(methyl methacrylate block styrene) (P(MMA-b-St)):...

Embodiment 3

[0081] 1. Synthesis of star-shaped hybrid arm polymers

[0082] (1) Synthesis of polymethyl methacrylate (PMMA): 12.5 g of methyl methacrylate, 0.455 g of RAFT reagent, 0.0205 g of AIBN, and 12.5 mL of toluene were charged into a flask. Perform freeze degassing several times. Polymerization was carried out at 70°C for 3 hours. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0083] (2) Synthesis of poly(methoxypolyethylene glycol acrylate) (P(PEGMEA)): 15 g of methoxypolyethylene glycol acrylate, 0.0455 g of RAFT reagent, 0.0205 g of AIBN, and 12.5 mL of toluene were charged into a flask. Perform freeze degassing several times. Polymerization was carried out at 70°C for 2 hours. Quench with liquid nitrogen. The mixed solution after polymerization is poured into petroleum ether to separate out linear polymer.

[0084] (3) Synthesis of poly(methyl methacrylate block styrene) (P(MMA-b-St))...

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Abstract

The invention relates to preparation of a silicon dioxide microsphere with a nonionic / anionic-combined-type surfactant as a soft template and belongs to preparation of silicon dioxide hybridized microspheres. The invention discloses a miktoarm star segmented copolymer with polyhedral oligomeric silsesquioxane as a core, which is prepared through polymerization in a manner of reversible addition-fragmentation chain transfer. The copolymer contains a hydrophilic poly(methoxyl polyethylene glycol acrylate) segment, a hydrophobic polymethyl methacrylate segment, a hydrophobic polystyrene segment, and the polyhedral oligomeric silsesquioxane core. The preparation of the mesoporous silicon dioxide material mainly includes a step of selectively volatilizing tetrahydrofuran with the miktoarm star segmented copolymer as the soft template, tetraethoxysilane as a silicon source and a tetrahydrofuran / hydrochloric acid solution as a mixture solvent. The silicon dioxide microsphere can form a robust spherical micelle, wherein the core is the polyhedral oligomeric silsesquioxane coated by the hydrophobic segments and an external layer is a comb-shaped PEGMEA chain segment. The silicon dioxide microsphere is 100-150 nm in diameter and can be used in a coating for improving anti-static, anti-adhesion and dispersing properties.

Description

technical field [0001] The invention belongs to the field of inorganic / organic hybrid materials, and relates to the preparation of silica hybrid microspheres, in particular to a preparation method using non-ionic / anion-bound surfactants as soft templates. Background technique [0002] Mesoporous microspheres have very high specific surface area, large pore volume, and low density, and are widely used in adsorption and separation, catalysis, ion exchange, micro-nano reactors and other fields. The synthesis of microspheres is generally based on the concept of template synthesis, and the templates used include soft templates and hard templates. The soft template method has fewer synthesis steps, is easy to synthesize on a large scale, and is widely used. Soft templates include surfactants and amphiphilic block copolymers. Due to the large molecular weight of block copolymers, it is easier to synthesize mesoporous materials with large pores. At the same time, the mesoscopic st...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00C08G81/02
CPCB82Y30/00B82Y40/00C01B33/18C01P2004/03C01P2004/32C01P2004/61C08G81/021
Inventor 张官云高树曦肖兴
Owner 广州赫尔普化工有限公司
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