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A temperature-sensitive nanogel material based on polyquaternary phosphonium salt ionic liquid and its preparation method

A technology of ionic liquids and nanogels, applied in the field of temperature-sensitive nanogel materials based on polyquaternary phosphonium salt ionic liquids and its preparation, and temperature-sensitive nanogel materials, which can solve application limitations, slow response speed, etc. question

Inactive Publication Date: 2016-02-10
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as a temperature-sensitive material, poly-N-isopropylacrylamide has a slow response speed, which limits its application.

Method used

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  • A temperature-sensitive nanogel material based on polyquaternary phosphonium salt ionic liquid and its preparation method
  • A temperature-sensitive nanogel material based on polyquaternary phosphonium salt ionic liquid and its preparation method
  • A temperature-sensitive nanogel material based on polyquaternary phosphonium salt ionic liquid and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Synthesis of quaternary phosphonium salt ionic liquid monomer PILB: Accurately weigh 4-vinylbenzyl chloride (1.5262g, 0.01mol) and triphenylphosphine (3.1476g, 0.012mol), mix well and pour into 100mL In the round bottom flask, add 50mL acetone as a solvent; then place it in an oil bath at 60°C, under N 2 Under the protection of reflux reaction for 48h. After the reaction is complete, pour the reaction mixture into 150 mL of diethyl ether to precipitate a white precipitate, filter it to obtain a white precipitate, wash it, and dry it in a vacuum oven at room temperature to obtain a white powder, which is 4-vinylbenzyl chloride Triphenylphosphonium ionic liquid PILB with a yield of 85%.

[0030] (2) Preparation of crosslinked nanogel CLPN based on polyquaternary phosphonium salt ionic liquid: Accurately weigh ethylene glycol dimethacrylate (EGDMA, 0.4955g, 2.5mmol), PILB (0.1037g, 0.25mmol), CTA1 (0.0308g, 0.1092mmol) and AIBN (0.0059g, 0.0364mmol), mixed evenly, po...

Embodiment 2

[0032] (1) Synthesis of quaternary phosphonium salt ionic liquid monomer PILB: same as Example 1.

[0033](2) Preparation of crosslinked nanogel CLPN based on polyquaternary phosphonium salt ionic liquid: Accurately weigh ethylene glycol dimethacrylate (EGDMA, 1.4866g, 7.5mmol), PILB (0.2075g, 0.5mmol), CTA2 (0.3752g, 0.1031mmol) and AIBN (0.0169g, 0.1031mmol), mixed evenly, poured into a 100mL round bottom flask, then added 30mL methanol as a solvent, mixed and placed in an oil bath at 70°C. N 2 Reflux reaction 7h under protection, the obtained yellow-blue solution is poured into the diethyl ether to separate out the product, filters, then puts in the vacuum oven and dries overnight, obtains the cross-linked nanogel CLPN based on the quaternary phosphonium salt ionic liquid, and the yield is 81.2%. Its structural expression is the same as before, wherein, g=73, m=5, k=73, R=Ph. Its phase transition temperature is 13°C, its hydrodynamic diameter is 35nm, and its particle si...

Embodiment 3

[0035] (1) Synthesis of PILD, a quaternary phosphonium salt ionic liquid monomer: Accurately weigh 4-vinylbenzyl chloride (1.5262g, 0.01mol) and tributylphosphine (2.4276g, 0.012mol), mix well and pour into 100mL In the round bottom flask, add 50mL acetone as a solvent; then place it in an oil bath at 60°C, under N 2 Under the protection of reflux reaction for 48h. After the reaction is complete, pour the reaction mixture into 150 mL of ether to settle a white precipitate, filter to obtain a white precipitate, wash it, and dry it in a vacuum oven at room temperature to obtain a white powder, which is 4-vinylbenzyltributyl Phosphonium-based ionic liquid PILD, the yield was 78.6%.

[0036] (2) Preparation of cross-linked nanogel CLPN based on polyquaternary phosphonium salt ionic liquid: Accurately weigh ethylene glycol dimethacrylate (EGDMA, 0.7433g, 3.75mmol), PILD (0.088g, 0.25mmol), CTA1 (0.0705g, 0.25mmol) and AIBN (0.0083g, 0.05mmol), mixed evenly, poured into a 100mL ro...

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Abstract

The invention discloses a temperature-sensitive nano gel material based on polyquaternary phosphonium salt ionic liquid, which belongs to the field of new materials. In the present invention, methanol is used as a solvent, azobisisobutyronitrile is used as an initiator, CTA1 or CTA2 is used as a chain transfer agent, and under the protection of N2, 4-vinylbenzyltriphenyl (butyl) phosphonium chloride ionic liquid is cross-linked derived from the reaction. The hydrodynamic diameter of the temperature-sensitive nanogel prepared by the present invention is between 20 and 90nm, the particle size distribution index is between 0.112 and 0.464, and within the temperature range of -5 to 13°C, macro gel and micro gel can be realized. The phase transition of the gel has reversible temperature responsiveness. After the surface is grafted and polymerized with N-isopropylacrylamide PNIPAm, it has a wide range of applications in drug release, immobilized enzymes, material separation, immunoassay and catalysis. prospect.

Description

technical field [0001] The invention relates to a temperature-sensitive nano gel material, in particular to a temperature-sensitive nano gel material based on a polyquaternary phosphonium salt ionic liquid and a preparation method thereof, belonging to the field of new materials. Background technique [0002] Ionic liquids (Ionic Liquids, ILs) refer to salts that are liquid at room temperature or near room temperature, mainly composed of organic cations and inorganic or organic anions, and they have many unique properties that are incomparable to other solvents. Compared with traditional liquid pure substances, ionic liquids are completely composed of ions; compared with conventional ionic pure substances, they are liquid at room temperature, have almost zero vapor pressure, are colorless and odorless, and have good chemical stability. , wide electrochemical stable potential window and temperature stable range, it is expected to replace traditional organic solvents as a clas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F230/02C08F2/38
Inventor 熊玉兵郭娜焦振乾李凤
Owner NORTHWEST NORMAL UNIVERSITY