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Temperature-sensitive nano gel material based on polyquaternary phosphonium salt ionic liquid and preparation method thereof

A technology of ionic liquids and nanogels, applied in the field of new materials, can solve problems such as application limitations and slow response speed

Inactive Publication Date: 2014-08-13
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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  • Temperature-sensitive nano gel material based on polyquaternary phosphonium salt ionic liquid and preparation method thereof
  • Temperature-sensitive nano gel material based on polyquaternary phosphonium salt ionic liquid and preparation method thereof
  • Temperature-sensitive nano gel material based on polyquaternary phosphonium salt ionic liquid and preparation method thereof

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 (1.5262 g, 0.01mol) and triphenylphosphine (3.1476g, 0.012mol), mix well and pour into 100 mL of round-bottomed flask, add 50 mL of 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 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-vinylbenzyl chloride Based triphenylphosphonium ionic liquid PILB, the yield was 85%.

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

Embodiment 2

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

[0033](2) Preparation of cross-linked nanogel CLPN based on polyquaternary phosphonium salt ionic liquid: Accurately weigh ethylene glycol dimethacrylate (EGDMA, 1.4866g, 7.5 mmol), PILB (0.2075g, 0.5 mmol), CTA2 (0.3752g, 0.1031mmol) and AIBN (0.0169 g, 0.1031mmol), mix well and pour into a 100 mL round bottom flask, then add 30 mL of methanol as a solvent, mix and place in an oil bath at 70°C , at 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 35 nm, and its parti...

Embodiment 3

[0035] (1) Synthesis of PILD, a quaternary phosphonium salt ionic liquid monomer: Accurately weigh 4-vinylbenzyl chloride (1.5262 g, 0.01mol) and tributylphosphine (2.4276 g, 0.012mol), mix well and pour into 100 mL of round-bottomed flask, add 50 mL of acetone as a solvent; then place it in an oil bath at 60°C, under N 2 Under the protection of reflux reaction for 48 h. After the reaction was complete, the reaction mixture was poured into 150 mL of diethyl ether to precipitate a white precipitate, which was filtered to obtain a white precipitate, washed, and dried at room temperature in a vacuum oven to obtain a white powder, which was 4-vinylbenzyltri Butylphosphonium 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, 3.75 mmol), PILD (0.088g, 0.25 mmol), CTA1 (0.0705g, 0.25mmol) and AIBN (0.0083 g, 0.05mmol), mi...

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Abstract

The invention discloses a temperature-sensitive nano gel material based on a polyquaternary phosphonium salt ionic liquid, and belongs to the field of new materials. With methanol as a solvent, azodiisobutyronitrile as an initiator and CTA1 or CTA2 as a chain transferring agent, and under the protection of N2, the temperature-sensitive nano gel material is obtained by carrying out a cross-linking reaction of a chlorinated 4-vinyl benzyl triphenyl butyl phosphonium ionic liquid. The hydrodynamic diameter of the prepared temperature-sensitive nano gel is 20 to 90 nm, the particle size distribution index is 0.112 to 0.464, and phase transformation of a macro gel and a micro gel can be achieved in a temperature range of -5 to 13 DEG C. The temperature-sensitive nano gel material has reversible temperature response, and has broad application prospects in drug release, enzyme immobilization, material separation, immunoassay, catalysis and other fields after the surface is grafted with polymerized N-isopropylacrylamide PNIPAm.

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 (ILs) refer to salts that are liquid at or near room temperature mainly composed of organic cations and inorganic or organic anions. They have many unique properties that cannot be compared with 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 class of green and environmentally fr...

Claims

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Application Information

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