Intelligent hydrogel synthesized from composite cross-linking agents, preparation method and application of intelligent hydrogel

A composite cross-linking agent and hydrogel technology, which is applied in the direction of pharmaceutical formulations, medical preparations of non-active ingredients, etc., can solve the problems of long response time of gel materials, improve biocompatibility, improve response speed, The effect of improving mechanical properties

Inactive Publication Date: 2013-12-11
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, although a lot of work has been done on the synthesis and application of smart macromolecules and macromolecular hydrogels, many corresponding physical and engineering problems are far from being solved, and the response time of most gel materials is still too long , the mechanical properties of the gel also need to be further improved, and the biocompatibility also needs to be further improved

Method used

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  • Intelligent hydrogel synthesized from composite cross-linking agents, preparation method and application of intelligent hydrogel
  • Intelligent hydrogel synthesized from composite cross-linking agents, preparation method and application of intelligent hydrogel
  • Intelligent hydrogel synthesized from composite cross-linking agents, preparation method and application of intelligent hydrogel

Examples

Experimental program
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Effect test

Embodiment 1

[0053] The preparation process of polyethylene glycol diacrylate (PEGDAc) used in Examples 3 to 6 is as follows: Take 6g of PEG and dissolve it in 50ml of dichloromethane, add 1ml of acrylic acid and 0.1g of 2-methylaminopyridine, mix well, and put it under the protection of argon. , another 1g of N,N-dicyclohexylcarbodiimide was dissolved in 20ml of dichloromethane, slowly added to the above solution under ice-cooling, and reacted at room temperature for 48h. The reaction solution was washed once with 1M hydrochloric acid solution, twice with saturated sodium carbonate solution, and three times with distilled water, dried over anhydrous magnesium sulfate, and then rotary evaporated to obtain polyethylene glycol diacrylate, which was designated as PEGDAc. Its H 1 NMR spectrum see figure 1 , resulting in:

[0054] δ=3.58~3.63(t,4H,-OCH 2 CH 2 ); δ=4.31~4.39(m,2H,-CH 2 ); δ=5.77~5.80,6.32~6.4(m,2H,=CH 2 ); δ=6.03~6.11(m,1H,=CH-).

Embodiment 2

[0056] The preparation process of polycaprolactone diacrylate (PCLDAc) used in implementation 3-6 is as follows: take 10g of polycaprolactone diol and dissolve it in 100ml of dichloromethane, add 1g of triethylamine, stir well, and Under protection, another 0.75 g of acryloyl chloride was mixed with 20 ml of dichloromethane, and slowly added dropwise to the above solution under ice bath, and reacted at 40° C. for 24 hours after the dropwise addition was completed. The reaction solution was washed once with 1M hydrochloric acid solution, twice with saturated sodium carbonate solution, and three times with distilled water, dried over anhydrous magnesium sulfate and then rotary evaporated to obtain polycaprolactone diacrylate, which was designated as PCLDAc. Its H 1 NMR spectrum see figure 2 , resulting in:

[0057] δ=1.31~1.35(m,2H,-CH2-);δ=1.58~1.61(m,2H,-CH 2 -); δ=2.26~2.31(m,2H,-CH 2 -); δ=3.8~3.81(t,2H,-CH 2 -C=O); δ=4.05~4.1(t,2H,-CH 2 -O-); δ=5.75~5.78,6.34~6.39(m,...

Embodiment 3

[0059] Weigh 0.0208g of PEGDAc, 0.0291g of PCLDac, and 0.1998g of N-isopropylacrylamide and dissolve them in 2ml of 1,4-dioxane, mix them uniformly by ultrasonication for 15 minutes, add 6mg of azobisisobutylcyanide, mix well and freeze Thaw cycle to remove oxygen, react at 60°C for 24 hours under the protection of argon, crush the reactor, soak the gel in distilled water for 4 days, change the water every day, remove unreacted particles to obtain the composite crosslinking agent intelligent hydrogel, cut into 10mm*5mm cylindrical small pieces are reserved, marked as N1.

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Abstract

The invention discloses an intelligent hydrogel synthesized from composite cross-linking agents, a preparation method of the intelligent hydrogel and an application of the intelligent hydrogel, and belongs to the field of preparation of the intelligent polymer hydrogel. The method provided by the invention is a method for preparing the intelligent thermo-sensitive N-isopropyl acrylamide hydrogel synthesized by polyethylene glycol diacrylate and polycaprolactone diacrylate as the composite cross-linking agents. The preparation method provided by the invention comprises the three steps: 1, preparing a polyethylene glycol macromolecule cross-linking agent; 2, preparing a polycaprolactone macromolecule cross-linking agent; and 3, preparing the thermo-sensitive N-isopropyl acrylamide hydrogel by taking the polyethylene glycol diacrylate and the polycaprolactone diacrylate as the composite cross-linking agent. The prepared N-isopropyl acrylamide hydrogel is good in mechanical strength, relatively high in response speed and good in biological capability, is degradable, and is expected to be used in the field of controlled release of drugs.

Description

technical field [0001] The invention belongs to the field of intelligent polymer hydrogel preparation, and in particular relates to a composite crosslinking agent intelligent hydrogel and its preparation method and application. Background technique [0002] Smart materials are functional materials that have a perception function, that is, a signal perception function (sensor function), and can draw conclusions (intelligence information processing function). Because of their intelligent behaviors that are sensitive to the external environment and can respond accordingly, smart materials have attracted increasing attention from all aspects. [0003] Smart polymer hydrogel is a representative class of smart polymer materials. It has the three-dimensional network structure of traditional gels and can respond to tiny physical and chemical stimuli in the environment, such as temperature, electric field, magnetic field, light, pH, ion Intensity, pressure, etc. are perceived, proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/06C08F220/54C08G65/48C08G63/91A61K47/34A61K47/14
Inventor 吕满庚李朝霞
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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