Preparation method for temperature-sensitive core-shell structured microspheres and application thereof in separation

A molecular weight, telechelic polymer technology, applied in the field of temperature-sensitive core-shell structure microspheres, can solve the problems of low monomer grafting rate, difficult control of molecular weight core-shell structure, high consumption of raw materials, etc. Good separation effect and complete reaction degree

Inactive Publication Date: 2013-03-20
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the methods they use are all synthesized by initiating polymerization and grafting on the surface of silica gel, or by copolymerization. The disadvantages are that the consumption of raw materials is large, the grafting rate of monomers is not high, and the molecular weight and its core-shell structure are not easy to control.

Method used

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  • Preparation method for temperature-sensitive core-shell structured microspheres and application thereof in separation
  • Preparation method for temperature-sensitive core-shell structured microspheres and application thereof in separation
  • Preparation method for temperature-sensitive core-shell structured microspheres and application thereof in separation

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Experimental program
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Effect test

Embodiment 1

[0017] like figure 1 As shown, N-isopropylacrylamide is a reactive monomer, azobisisobutyronitrile is used as an initiator, and mercaptopropyltriethoxysilane is dissolved in DMF as a molecular weight regulator (see Table 1 for specific dosage) , the above mixture was reacted at 70° C. for 10 h under the protection of nitrogen, and the product was rotary evaporated at 70° C. After concentration, the polymer was precipitated with diethyl ether as a precipitating agent. The polymer was further purified by repeated dissolution-sedimentation with THF and ether.

[0018] Table 1 Synthetic formula and results of semi-telechelic polymer

[0019]

Embodiment 2

[0021] Add the above-mentioned macromolecular product and silica gel particles into toluene solvent, add a certain amount of pyridine as a reaction auxiliary agent, and mix well. Under the protection of nitrogen, react at 110°C for 10h. The product is centrifugally settled, and the obtained composite particles are repeatedly extracted with deionized water to remove ungrafted macromolecular aggregates, and then repeatedly washed with methanol and ultrapure water in sequence. The product was dried under vacuum at room temperature to obtain a white powdery solid.

[0022] Table 2 The synthetic grafting ratio of the composites as a function of time

[0023]

Embodiment 3

[0025] Surface modified silica gel at 350kg / cm 2 Under the pressure of 100%, the mixed solvent of methanol and water (1:1) was filled into a stainless steel column (150mm × 4.6mm) as a homogenizer, and then equilibrated with deionized water for 4h; the steel column was connected to the HPLC system (Waters 1525 Binany HPLC Pump, Waters 2996 Potodiode Array Detector, Waters 717Plus Autosampler). A mixture of three aqueous solutions of naphthalene derivatives was used as a solute, a mixture of water / methanol in a volume ratio of 9:1 was used as a mobile phase, and chromatographic separation was performed at a flow rate of 1.0 mL / min. The concentrations of the three naphthalene derivatives were 4 mg / mL for naphthalene acetic acid; 6 mg / mL for naphthylamine; and 5.7 mg / mL for naphthol. Detected at UV 215nm, controlled different temperatures to observe the elution behavior of the three substances. The temperature is controlled by a column thermostat, and its temperature fluctuatio...

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Abstract

A preparation method for temperature-sensitive core-shell structured microspheres and an application thereof in separation. According to the present invention, first mercaptopropyl triethoxysilane (MPT) and N-isopropyl acrylamide are reacted to generate semi-telechelic polymers, then the semi-telechelic polymers are coupled with ultrafine colloidal silica particles, so composite particles with poly-N-isopropyl acrylamide as the shells and colloidal silica particles as the cores are prepared. Differential scanning calorimetry tests show that the composite particles are temperature-sensitive. The prepared composite particles are used as a stationary phase in high pressure liquid chromatography, and water is used as a main ingredient of a mobile phase, and naphthalene derivatives are separated successfully through the control of column temperatures, achieving good separation effect.

Description

Technical field: [0001] The invention prepares a novel temperature-sensitive core-shell structure microsphere and uses it for the separation of organic substances, belonging to the field of novel functional materials. Background technique: [0002] The synthesis and performance research of temperature-sensitive polymers and inorganic substances such as composite materials have been reported in the literature, but most of the inorganic substances used are montmorillonite, inorganic salts or nano-inorganic materials. Silica gel is currently the most widely used high-performance liquid chromatography. Stationary Phase. This is because in addition to the advantages of good mechanical strength, easy-to-control pore structure and specific surface area, good chemical stability and thermal stability, and specific surface chemical reaction, silica gel has another outstanding advantage: its surface Rich in silanol, which is the basis for surface chemical bonding or modification of si...

Claims

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Application Information

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IPC IPC(8): C08F120/54C08F2/38C08F8/42B01J20/28B01J20/281B01D15/08
Inventor 陶蕾倪才华朱毅张丽萍
Owner JIANGNAN UNIV
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