Preparation method of high-strength hydrogel

A hydrogel, high-strength technology, applied in the field of hydrogels, can solve the problems of complex and time-consuming preparation process, restricting the application of high-strength hydrogels, etc., and achieves green and safe preparation process, short preparation process time, and energy consumption. small effect

Inactive Publication Date: 2014-04-23

HENAN POLYTECHNIC UNIV

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Problems solved by technology

[0004] Although some important achievements have been made in the design and preparation of high-strength hydrogels, the preparation process of high-strength hydrogels is gener...

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Abstract

The invention relates to a high-strength hydrogel and a preparation method thereof. The preparation method comprises the steps of directly mixing a polymer, a monomer, an initiator, a cross-linking agent and water once, dissolving all the substances to form a homogeneous solution under a certain simulation condition, and then initiating and polymerizing by using heat or light to obtain the high-strength hydrogel, wherein the polymer is needed for preparation of the hydrogel and used for forming a first double network of a dual-network hydrogel; the monomer is used for polymerizing and forming a second double network of the dual-network hydrogel; the initiator is used for initiating the monomer to be polymerized; the cross-linking agent is used for performing cross-linking reaction in a monomer polymerizing process so as to form the second double network. According to the preparation method, a one-pot method is used for preparing the high-strength hydrogel, so that the method is simple and practicable; the prepared high-strength hydrogel has the characteristics of high strength and high toughness; a tensile strength of the gel is 0.6-1.2MPa, a tensile modulus is 100-200 KPa and a tensile strain reaches 1000-2680%; the prepared high-strength hydrogel can be widely applied to the fields of tissue repair, artificial organ, drug sustained release, sensors and the like.

Technology Topic

Polymer chemistryDouble network +3

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Examples

Experimental program(11)

Example Embodiment

[0027] A method for preparing a high-strength hydrogel. The specific preparation method is that the high-strength hydrogel adopts a "one-pot cooking" method, that is, the first step required for the preparation of the hydrogel to form a double network gel The polymer of the network, the monomer used to polymerize to form the second heavy network of the double network hydrogel, the initiator used to initiate the polymerization of the monomer, and the crosslinking reaction to occur simultaneously during the polymerization of the monomer to form the second The cross-linking agent of the heavy network is directly mixed with water at one time, and all the substances are dissolved to form a homogeneous solution under certain stimulating conditions, and then heat or light is used to initiate polymerization to obtain a high-strength hydrogel;

[0028] The polymer used to form the first network of the double network gel is agar, agarose, gelatin, collagen, fibrin, alginate, hyaluronate, chondroitin sulfate, carrageenan, gellan One or a combination of two or more of gum, guar gum, sesame gum, chitosan, and oxidized starch;

[0029] The monomers used to polymerize to form the second network of the double network hydrogel are acrylamide, N,N'-dimethylacrylamide, acrylic acid and its salts, methacrylic acid and its salts, and methacrylic acid. One or a combination of two or more of octaester, methacrylate laurate, and polyethylene glycol diacrylate;

[0030] The initiator used to initiate monomer polymerization is 2,2-diethoxyacetophenone, 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, 1-hydroxyl One of cyclohexylpropiophenone, 2-oxoglutaric acid, ammonium persulfate, potassium persulfate;

[0031] The crosslinking agent used to cause the crosslinking reaction to occur simultaneously during the polymerization of the monomers to form the second heavy network is N,N'-methylenebisacrylamide, ethylene glycol dimethacrylate, dimethyl One of diethylene glycol acrylate and polyethylene glycol diacrylate;

[0032] The certain stimulating conditions are heating, light, and pH.

[0033] A method for preparing high-strength hydrogel, the preparation method is preferably the following scheme; the specific preparation steps are:

[0034] Step 1. Weigh the polymer, monomer, initiator, crosslinking agent, other additives and water in the reactor so that the polymer concentration is 1-100 mg/mL and the monomer concentration is 1-5 mol/L 、The molar concentration percentage of the initiator relative to the monomer is 0.01-5 mol%, and the molar concentration percentage of the crosslinking agent to the monomer is 0-5 mol%. Then replace the oxygen in the reactor with nitrogen or argon to obtain a mixture The reaction solution;

[0035] Step 2. Stir the mixed reaction solution in the reactor at 60-90℃ for 5-10 min to form a homogeneous transparent clear solution; irradiate the obtained transparent clear solution under a 365 nm UV lamp for 1-2 h. Produce high-strength hydrogel.

[0036] The preparation method can choose to add auxiliary additives when mixing the materials required for the preparation of the hydrogel. The auxiliary additives are one of surfactants, divalent metal cations, trivalent metal cations, and small molecule salts. One or a combination of two or more; the surfactant is sodium dodecyl sulfonate, sodium dodecyl sulfate or cetyltrimethylammonium bromide; the divalent metal cation is Ca 2+ , Cu 2+ , Zn 2+ , Co 2+ , Sr 2+ Or Ba 2+; The trivalent metal cation is Fe 3+ , Al 3+ Or Eu 3+ The small molecule salt is NaCl or NaSCN; the total amount added is 0-5 mol/L.

Example Embodiment

[0037] Example 1

[0038] Mix 20 mg agar, 2400 mg acrylamide, 0.0575 g 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, 78 μL N,N'-methylenebisacrylamide solution ( 20 mg/mL) was accurately weighed and added to the reactor, and then 10 mL of deionized water was added. Seal the reaction liquid and circulate the oxygen and nitrogen flushing three times, at 90~95 o Heat and stir in the oil bath or water bath of C for 5-10 minutes to form a homogeneous transparent clear solution, then pour the solution into the reaction mold and cool it to room temperature to form agar gel. After the above agar gel is polymerized under 365 nm ultraviolet light for 1 h, it can be obtained as figure 1 , 2 , 3, 4 shows the high-strength hydrogel (the gel can be bent, knotted, compressed and stretched without breaking). The stress-strain curve of the tensile test of Agar/PAM DN gel is as follows: Figure 5 As shown in the figure, a is the stress-strain curve of the high-strength hydrogel of this embodiment, and b is the stress-strain curve of the polyacrylamide hydrogel; the tensile strength of the high-strength hydrogel of this embodiment is 1 MPa, a tensile modulus of 120 KPa, and a breaking elongation of 2000%. The mechanical properties of the gel are significantly better than those of polyacrylamide hydrogel (PAM gel).

Example Embodiment

[0039] Example 2

[0040] 50 mg gelatin, 2000 mg acrylamide, 29 μL N,N'-methylenebisacrylamide solution (20 mg/mL) were accurately weighed and added to the reactor, and then 10 mL deionized water was added. After the reaction liquid is sealed, the oxygen and nitrogen are circulated three times, at 60 o Heat and stir in the oil bath or water bath of C for 5-10 min to form a homogeneous transparent clear solution. Add 120 μL of ammonium persulfate or potassium persulfate aqueous solution (20 mg/mL) and pour the solution into the reaction mold to make Of 60 o C reacts for 2 h and then at 4 o C cool down for 0.5 h. The tensile strength is 1.2 MPa, the tensile modulus is 146 KPa, the elongation at break is 1740%, the compressive strength is about 40 MPa, the compressive modulus is about 155 KPa, the compressive strain is 96%, and the toughness of the gel reaches 800 J/m. 2.

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PUM

Property	Measurement	Unit
Tensile strength	1.0	mPa
Tensile strength	1.2	mPa
Tensile modulus	146.0	kPa
tensile		MPa
Particle size		Pa
strength	10

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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine

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