Preparation method of high-strength nano-composite hydrogel with rapid dual responses of pH and temperature

A nano-composite, high-strength technology, applied in the field of preparation of nano-composite hydrogels, can solve the problems of poor mechanical properties of hydrogel products, higher than 40 ° C, and no value of sustained drug release.

Inactive Publication Date: 2014-09-24
HUNAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents CN101215350A, CN101319019A and CN101161689B also disclose the preparation of nanocomposite temperature-sensitive hydrogels with modified inorganic nanoclays (such as sodium pyrophosphate-modified lethonite, hectorite) as physical cross-linking agents, but do not involve pH response and dual responsive hydrogels
[0010] And DMAEMA is also widely used in the synthesis of multi-response gels. Its synthesis methods include cross-linking with chemical cross-linking agent BIS and polymerization by ultraviolet cross-linking. However, the mechanical properties of these hydrogel products are still poor. And the lowest critical transition temperature LCST temperature is higher than 40 ℃, this temperature is higher than the human body temperature and does not have the value of being used for drug sustained release

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Prepare the pre-solution: dissolve 4g of dimethylaminoethyl methacrylate, 0.52g of nano-lithium diatomaceous earth, 0.08g of N,N'-methylenebisacrylamide, and 0.04g of sodium pyrophosphate in 24ml of water and put them together In a transparent flask, under the protection of nitrogen, stir in an ice bath at 0°C for 60 minutes until uniform and transparent, then add 0.48 g of nanocellulose whiskers and stir for 30 minutes, then ultrasonically oscillate for 10 minutes until uniform, wrap the flask with black cloth until it is opaque Light, add 0.02g photoinitiator diketoglutaric acid, stir in an ice bath for 10 minutes, transfer to a test tube and seal;

[0033] (2) Place the sealed test tube containing the above-mentioned pre-polymerization solution in front of a 360nm wavelength ultraviolet light source, the distance between the test tube and the light source is 10cm, and the pre-polymerization solution is irradiated under ultraviolet light for 30 minutes;

[0034] (...

Embodiment 2

[0038] (1) Prepare the pre-solution: Dissolve 4.4g dimethylaminoethyl methacrylate, 0.87g nano-lithium diatomaceous earth, 0.066g N,N'-methylenebisacrylamide, and 0.067g sodium pyrophosphate in 24ml water and mix Place in a transparent flask, stir in an ice bath at 0°C under nitrogen protection for 60 minutes until uniform and transparent, then add 0.96 g of nanocellulose whiskers and stir for 30 minutes, then ultrasonically oscillate for 10 minutes until uniform, wrap the flask with black cloth until it is not Light transmission, add 0.022g photoinitiator diketoglutaric acid, stir in ice bath for 10 minutes, transfer to test tube and seal;

[0039] (2) Place the sealed test tube containing the above-mentioned pre-polymerization solution in front of a 360nm wavelength ultraviolet light source, the distance between the test tube and the light source is 10cm, and the pre-polymerization solution is irradiated under ultraviolet light for 30 minutes;

[0040] (3) Take out the conta...

Embodiment 3

[0044] (1) Prepare the pre-solution: dissolve 4.2g dimethylaminoethyl methacrylate, 1.31g nano-lithium diatomaceous earth, 0.04g N,N'-methylenebisacrylamide, 0.1g sodium pyrophosphate in 24ml water and mix Place in a transparent flask, stir in an ice bath at 0°C under nitrogen protection for 60 minutes until uniform and transparent, then add 1.1 g of nanocellulose whiskers and stir for 30 minutes, then ultrasonically oscillate for 15 minutes until uniform, wrap the flask with black cloth until not Light transmission, add 0.04g photoinitiator diketoglutaric acid, stir in ice bath for 10 minutes, transfer to test tube and seal;

[0045] (2) Place the sealed test tube containing the above-mentioned pre-polymerization solution in front of a 360nm wavelength ultraviolet light source, the distance between the test tube and the light source is 10cm, and the pre-polymerization solution is irradiated under ultraviolet light for 30 minutes;

[0046] (3) Take out the container in (2) and...

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Abstract

The invention relates to a preparation method of high-strength nano-composite hydrogel capable of rapidly responding to pH and temperature. The preparation method taking dimethylaminoethyl methacrylate as a monomer, inorganic nanometer clay and N,N'-methylenebisacrylamide as co-crosslinking agents, and a nanometer cellulose whisker as a gel composite reinforcer comprises the following steps of: stirring the components, carrying out uniform ultrasonic oscillation, carrying out photo-initiation free radical polymerization in 0 DEG C ice-bath, then reacting at -18 DEG C for 24 hours to obtain the final gel product. The hydrogel prepared by the method has the dual responses of temperature and pH and excellent mechanical performance and can rapidly swell and deswell; and the lowest transformation temperature of the hydrogel is close to temperature of human bodies; raw materials are cheap; the preparation method is simple; and the high-strength nano-composite hydrogel has the potential of application in fields such as sustained release of medicines and tissue engineering.

Description

technical field [0001] The invention belongs to a method for preparing a hydrogel, in particular to a method for preparing a nanocomposite hydrogel with high mechanical strength, which can produce rapid response to changes in ambient temperature and pH value, thereby producing volume transformation. Background technique [0002] Polymer gel refers to a system composed of a three-dimensional network structure of polymer compounds and a solvent, in which the polymers are connected by van der Waals force, chemical bond force, physical winding force, hydrogen bond force, etc. Since it is a three-dimensional network structure, it cannot be dissolved by solvents, and at the same time, it can be dispersed in solvents and can maintain a certain shape. Although the solvent cannot dissolve the polymer with a three-dimensional network structure, the solvophilic group in the polymer compound can be affected by the solvent to swell the polymer, which is also the reason for the formation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/34C08F2/48C08F2/44C08K9/02C08K3/34C08K3/32
Inventor 陈一
Owner HUNAN UNIV OF TECH
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