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Method for preparing temperature-sensitive modified nanosilicon dioxide complexes having different critical response temperatures

A technology of nano-silica and composites, which is applied in the field of preparing temperature-sensitive modified nano-silica composites with different critical response temperatures, which can solve the problems of harsh reaction conditions, poisonous catalysts, and easy oxidation, and achieve easy The effects of preparation, cost reduction, and wide range of applications

Active Publication Date: 2014-10-29
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned technologies still have disadvantages such as harsh reaction conditions, toxic or easily oxidized catalysts, and unadjustable temperature response of temperature-sensitive composite materials.

Method used

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  • Method for preparing temperature-sensitive modified nanosilicon dioxide complexes having different critical response temperatures
  • Method for preparing temperature-sensitive modified nanosilicon dioxide complexes having different critical response temperatures

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0034] This implementation pre-prepared temperature-sensitive modified nano-SiO with LCST of 26 °C 2 Composite, calculate according to formula (1) according to the LCST of complex:

[0035]LCST P =∑LCST Pi W i (1)

[0036] Select poly-2-methyl-2-acrylic acid-2-(2-methoxyethoxy)ethyl ester whose LCST is 26°C and molecular weight is 200 as a monomer, and the calculated LCST p is 26°C.

[0037] (1) At room temperature, dissolve 18ml of tetraethyl orthosilicate in 300ml of absolute ethanol, then add 20ml of concentrated ammonia water into the system drop by drop with a constant pressure dropping funnel, and react at 500rpm for 5h to obtain nano-SiO 2 suspension solution.

[0038] (2) At a speed of 500rpm, add 18ml of silane coupling agent γ-aminopropyltriethoxysilane to the above mixed solution, heat to reflux, and react for 6h to obtain a coupling agent-modified nano-SiO 2 The suspension was cooled to room temperature, filtered with suction, washed with ethanol and wate...

Embodiment 2

[0041] This implementation pre-prepared temperature-sensitive modified nano-SiO with LCST of 65 °C 2 Composite, calculate according to formula (1) according to the LCST of complex:

[0042] LCST P =∑LCST Pi W i (1)

[0043] Select polyethylene glycol methacrylate with LCST at 65°C and molecular weight of 300 as the monomer, and calculate the LCST p is 65°C.

[0044] (1) At room temperature, dissolve 10ml of butyl orthosilicate and 10mL of methyl orthosilicate in 300mL of 95% ethanol, then add 25ml of monoethanolamine dropwise into the system with a constant pressure dropping funnel, and react at 700rpm 10h, get nano-SiO 2 suspension solution.

[0045] (2) At 700rpm, add 18ml of silane coupling agent N-β(aminoethyl)-γ-aminopropyltriethoxysilane to the above mixed solution, heat to reflux, and react for 10h to obtain coupling agent Modified nano-SiO 2 The suspension was cooled to room temperature, filtered with suction, washed with ethanol and water at least three ti...

Embodiment 3

[0049] This implementation pre-prepared temperature-sensitive modified nano-SiO with LCST of 40 °C 2 Composite, calculate according to formula (1) according to the LCST of complex:

[0050] LCST P =∑LCST Pi W i (1)

[0051] Select polyethylene glycol methacrylate with a molecular weight of 300 at LCST of 65°C and N-isopropylacrylamide with a LCST of 32°C as monomers. After calculation, the molecular weight of polyethylene glycol methacrylate with a molecular weight of 300 The mass percent is 24.24%, the mass percent of N-isopropylacrylamide is 75.76%, the LCST obtained p is 40°C.

[0052] (1) At room temperature, dissolve 20ml of butyl orthosilicate in 300mL of n-butanol, then add 28ml of triethanolamine dropwise into the system with a constant pressure dropping funnel, and react at 800rpm for 10h to obtain nano-SiO 2 suspension solution.

[0053] (2) At 800rpm, add 20ml of silane coupling agent N-β(aminoethyl)-γ-aminopropyltrimethoxysilane into the above mixed solut...

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Abstract

A method for preparing temperature-sensitive modified nanosilicon dioxide complexes having different critical response temperatures comprises the steps: adding an alkaline substance into a mixed solution of an SiO2 precursor and a solvent, after reaction, adding a silane coupling agent, carrying out a reaction at a reflux temperature, carrying out suction filtration, washing, and drying to obtain an SiO2-NH2 powder; dispersing the SiO2-NH2 powder into toluene, adding an initiator and an acid binding agent, carrying out a reaction, carrying out suction filtration, washing, and drying to obtain an SiO2-Br powder; dispersing the SiO2-Br powder into dichloromethane, carrying out ultrasonic dispersion, adding a catalyst and a ligand, introducing nitrogen gas, adding a monomer and deionized water with stirring, dripping a reducing agent, carrying out a polymerization reaction, carrying out suction filtration, washing, and drying; and carrying out soxhlet extraction on the obtained sample with ethanol, and drying to obtain the temperature-sensitive nano modified SiO2 complexes. The method has mild reaction conditions, and prepares the products having different critical response temperatures.

Description

technical field [0001] The invention relates to a method for preparing temperature-sensitive modified nano silicon dioxide composites with different critical response temperatures. Background technique [0002] Thermosensitive polymers refer to polymers that can change the conformation of their molecular chains in response to slight changes in ambient temperature. There is a critical response temperature (LCST) in the temperature-sensitive polymer in the solution. When the temperature is lower than the LCST, the polymer is in a stretched state. When the temperature is higher than the LCST, the polymer chain undergoes a coil-to-globule transformation, forming a precipitate . The most widely studied temperature-sensitive polymer is poly-N-isopropylacrylamide (PNIPAAm), whose LCST is about 32°C, which is close to human body temperature. The lower and narrower LCST limits the scope of use of PNIPAAm to some extent. Polyether is also a kind of temperature-sensitive polymer, wh...

Claims

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Application Information

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IPC IPC(8): C08L51/10C08L33/14C08K9/04C08K9/06C08K3/36C08F292/00C08F220/54
Inventor 杜志平孙晓峰台秀梅王万绪王国永
Owner CHINA RES INST OF DAILY CHEM IND