CN108329497B - Moisturizing and anti-freezing hydrogel and preparation method thereof - Google Patents

Moisturizing and anti-freezing hydrogel and preparation method thereof Download PDF

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CN108329497B
CN108329497B CN201810055103.6A CN201810055103A CN108329497B CN 108329497 B CN108329497 B CN 108329497B CN 201810055103 A CN201810055103 A CN 201810055103A CN 108329497 B CN108329497 B CN 108329497B
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hydrogel
gel
moisturizing
antifreeze
solvent
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CN108329497A (en
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周学昌
陈繁
周丹
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Shenzhen University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F251/00Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/02Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2305/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/04Alginic acid; Derivatives thereof

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Abstract

The invention discloses an anti-freezing moisturizing gel and a preparation method thereof, wherein the method comprises the following steps: step A, preparing hydrogel; and step B, soaking the prepared hydrogel in an antifreeze moisturizing solvent to replace the antifreeze moisturizing solvent with water in the hydrogel to obtain the antifreeze moisturizing gel. After the hydrogel is prepared, the water in the hydrogel is replaced with the soaked solvent by a solvent replacement method. That is, the hydrogel is soaked in a solvent for freezing and moisture retention, such as glycerol, ethylene glycol, etc. The hydrogel is changed into the composition of a mixed system of the solvent and the water for freezing and moisture retention by exchanging the solvent and the water in the hydrogel, and the prepared gel has excellent moisture retention and freezing resistance.

Description

Moisturizing and anti-freezing hydrogel and preparation method thereof
Technical Field
The invention relates to the field of hydrogel, in particular to moisturizing and anti-freezing hydrogel and a preparation method thereof.
Background
The hydrogel has good stretchability, flexibility and adjustability, so that the hydrogel has wide effects in aspects of tissue engineering, drug delivery and the like. However, the 90% water content of the hydrogel makes it difficult to maintain the hydrogel in the air for a long period of time and to have freezing resistance at low temperatures. In many documents, the anti-freeze and moisturizing properties of hydrogels are increased by adding anti-freeze agents or humectants separately during the preparation of the hydrogels. For example, organic solvents are rendered frost resistant by the addition of a two-phase frost resistant solvent-ethylene glycol/water solution during the preparation of the hydrogel; it is also known to add glycerin to the hydrogel during the preparation process to make the hydrogel moisture-retaining at a certain temperature. In the above methods, the characteristics of the gel are changed by changing the manufacturing process of the gel, but the method requires controlling the amount of the anti-freezing agent or the humectant, is complicated to operate, and can be operated only on a single gel.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a moisturizing and anti-freezing hydrogel and a preparation method thereof, and aims to solve the problems that the prior method needs to control the dosage of an anti-freezing agent or a humectant, is complex to operate, and can only operate on a single gel.
The technical scheme of the invention is as follows:
a method for preparing a freeze resistant moisturizing gel, comprising:
step A, preparing hydrogel;
and step B, soaking the prepared hydrogel in an antifreeze moisturizing solvent to replace the antifreeze moisturizing solvent with water in the hydrogel to obtain the antifreeze moisturizing gel.
The preparation method of the anti-freezing moisturizing gel comprises the step of preparing a hydrogel from sodium alginate-acrylamide hydrogel, agar-acrylamide hydrogel, sodium alginate-chitosan hydrogel or PVA-PEG hydrogel.
The preparation method of the antifreeze moisturizing gel comprises the following steps of preparing an antifreeze moisturizing solvent from glycerol, ethanol, sorbitol, dimethyl sulfoxide/water binary solution, CaCl2Solution or glycol.
The preparation method of the anti-freezing moisturizing gel comprises the step of preparing an anti-freezing moisturizing gel, wherein the anti-freezing moisturizing solvent is glycerol.
The preparation method of the anti-freezing moisturizing gel comprises the step of soaking for 0.5-6 hours.
The preparation method of the anti-freezing moisturizing gel comprises the following steps of preparing a hydrogel, and preparing a gel matrix from the hydrogel and the anti-freezing moisturizing gel.
The preparation method of the antifreeze moisturizing gel comprises the following steps: dissolving sodium alginate and acrylamide in deionized water, sequentially adding N, N-methylene bisacrylamide and N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and injecting saturated calcium sulfate solution; pouring into a template, and irradiating and molding under ultraviolet light to obtain the sodium alginate-acrylamide hydrogel.
The preparation method of the anti-freezing moisturizing gel comprises the following steps of (1-3): (5-10).
The preparation method of the anti-freezing moisturizing gel comprises the step of irradiating for 40-50min under the ultraviolet light of 245nm for molding.
The invention discloses an antifreeze moisturizing gel, which is prepared by adopting the preparation method of the antifreeze moisturizing gel.
Has the advantages that: the invention prepares the moisture-keeping antifreeze gel by a solvent replacement method, namely after preparing the hydrogel, the prepared hydrogel is soaked in the antifreeze moisture-keeping solvent, and the hydrogel is changed into the composition of a mixed system of the solvent with antifreeze moisture-keeping property and water by exchanging the solvent with the water in the hydrogel, so that the prepared gel has excellent moisture-keeping property and antifreeze property. The method does not need to control the dosage of the anti-freezing moisturizing solvent, is simple to operate, and can be used for operating various gels.
Drawings
FIG. 1 is a diagram showing the relationship between the mass ratio of a gel soaked in glycerin for different time periods in air and the change of the mass ratio in air with time.
Detailed Description
The invention provides a moisturizing and anti-freezing hydrogel and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a preparation method of an antifreeze moisturizing hydrogel, which comprises the following steps:
step A, preparing hydrogel;
and step B, soaking the prepared hydrogel in an antifreeze moisturizing solvent to replace the antifreeze moisturizing solvent with water in the hydrogel to obtain the antifreeze moisturizing hydrogel.
In the prior art, an antifreeze agent or a humectant is added separately in the process of preparing hydrogel to improve the antifreeze and moisture retention characteristics of the hydrogel. However, the existing method needs strict control of the dosage of the antifreeze or the humectant, has complex operation and can only operate on a single gel. The invention is that after preparing hydrogel, the water in the hydrogel is replaced with the soaked solvent by a solvent replacement method. That is, the hydrogel is soaked in a solvent for freezing and moisture retention, such as glycerol, ethylene glycol, etc. The hydrogel is changed into the composition of a mixed system of the solvent and the water for freezing and moisture retention by exchanging the solvent and the water in the hydrogel, so that the prepared gel has excellent moisture retention and freezing resistance. Compared with the prior art, the method disclosed by the invention does not need to control the dosage of the anti-freezing and moisturizing solvent, is simple to operate, and can be used for operating various gels.
Specifically, the hydrogel may be a sodium alginate-acrylamide hydrogel, an agar-acrylamide hydrogel, a sodium alginate-chitosan hydrogel, a PVA-PEG hydrogel, or the like, without being limited thereto.
Specifically, the antifreeze moisture-keeping solvent is glycerol, ethanol, sorbitol, dimethyl sulfoxide/water binary solution, CaCl2The solution or glycol and the like are not limited thereto. The solvent has the antifreezing and moisturizing performances, and the antifreezing and moisturizing gel can be obtained by treating the hydrogel with the solvent.
The invention changes the frost resistance and moisture retention performance of the gel by controlling the soaking time. Preferably, the soaking time is 0.5-6 h. Within the soaking time range, the gel has better freezing resistance and moisture retention performance, and the longer the soaking time of the solvent is, the better the freezing resistance and moisture retention performance is.
The present invention will be further described below by taking sodium alginate-acrylamide hydrogel as an example.
The first step is as follows: the mass ratio of (1-3): and (5-10) dissolving sodium alginate and acrylamide in deionized water, sequentially adding 80-100 uL of N, N-methylene bisacrylamide and 8-12 uL of N, N, N ', N' -tetramethyl ethylenediamine, uniformly stirring, and slowly injecting 4-6 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 40-50min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel for one night, and then pouring the uniform gel into 60-100 mL of glycerol solution to ensure that water molecules and glycerol in the sodium alginate-acrylamide hydrogel are fully replaced. In the hydrogel, glycerol molecules enter the gel, thereby changing the properties of the hydrogel and enabling the hydrogel to have freezing resistance and moisture retention. The soaking time is 0.5-6 h.
The third step: after the gel is soaked in the glycerol, the gel is placed in a low-temperature reactor for an anti-freezing test, and the gel can still be bent at a low temperature through the test.
The invention prepares the moisturizing antifreeze hydrogel by a solvent displacement method, namely after preparing the sodium alginate-acrylamide hydrogel, the prepared hydrogel is soaked in an antifreeze moisturizing solvent glycerol, and the antifreeze and moisturizing performances of the gel are changed by controlling the soaking time. Finally, it was found that hydrogels soaked in glycerol did not lose water after prolonged exposure to air and still have flexural properties at-50 ℃. When the above glycerol was replaced with ethylene glycol without changing other conditions, it was finally found that the hydrogel soaked in ethylene glycol did not lose water after long-term exposure to air and still had flexural properties at-70 ℃.
The invention also provides an antifreeze moisturizing gel, wherein the antifreeze moisturizing gel is prepared by the preparation method of the antifreeze moisturizing gel.
The present invention will be described in detail below with reference to examples.
Example 1
The first step is as follows: mixing the components in a mass ratio of 1: dissolving sodium alginate and acrylamide of 3 in deionized water, sequentially adding 80 uL of N, N-methylene bisacrylamide and 8 uL of N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and slowly injecting 5 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 45 min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel overnight, then pouring the uniform gel into 100 mL of glycerol, and soaking for 0 min. So that the water molecules and the glycerol are fully replaced.
The third step: the soaked gel was taken out for moisture retention and freeze resistance tests.
Example 2
The first step is as follows: mixing the components in a mass ratio of 1: dissolving sodium alginate and acrylamide of 3 in deionized water, sequentially adding 80 uL of N, N-methylene bisacrylamide and 8 uL of N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and slowly injecting 5 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 45 min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel overnight, then pouring the uniform gel into 100 mL of glycerol, and soaking for 10 min. So that the water molecules and the glycerol are fully replaced.
The third step: the soaked gel was taken out for moisture retention and freeze resistance tests.
Example 3
The first step is as follows: mixing the components in a mass ratio of 1: dissolving sodium alginate and acrylamide of 3 in deionized water, sequentially adding 80 uL of N, N-methylene bisacrylamide and 8 uL of N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and slowly injecting 5 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 45 min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel overnight, then pouring the uniform gel into 100 mL of glycerol, and soaking for 20 min. So that the water molecules and the glycerol are fully replaced.
The third step: the soaked gel was taken out for moisture retention and freeze resistance tests.
Example 4
The first step is as follows: mixing the components in a mass ratio of 1: dissolving sodium alginate and acrylamide of 3 in deionized water, sequentially adding 80 uL of N, N-methylene bisacrylamide and 8 uL of N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and slowly injecting 5 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 45 min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel overnight, then pouring the uniform gel into 100 mL of glycerol, and soaking for 40 min. So that the water molecules and the glycerol are fully replaced.
The third step: the soaked gel was taken out for moisture retention and freeze resistance tests.
Example 5
The first step is as follows: mixing the components in a mass ratio of 1: dissolving sodium alginate and acrylamide of 3 in deionized water, sequentially adding 80 uL of N, N-methylene bisacrylamide and 8 uL of N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and slowly injecting 5 mL of saturated calcium sulfate solution by using a needle. Pouring into a template, and irradiating under ultraviolet light of 245nm for 45 min for molding to obtain the sodium alginate-acrylamide hydrogel.
The second step is that: and (3) uniformly placing the prepared sodium alginate-acrylamide hydrogel overnight, then pouring the uniform gel into 100 mL of glycerol, and soaking for 60 min. So that the water molecules and the glycerol are fully replaced.
The third step: the soaked gel was taken out for moisture retention and freeze resistance tests.
The test results were as follows:
1. FIG. 1 is a graph showing the weight change of the exposed gel in the air after the immersion in glycerol of examples 1 to 5 (mass ratio is the ratio of the weight of the gel after the exposure to the weight of the gel before the exposure), and it can be seen that the hydrogel can surely retain moisture by the solvent replacement method, and the longer the immersion time of the solvent, the better the moisture retention.
2. The gels of examples 1-5 were tested for freezing resistance after immersion in glycerol and were placed in a low temperature reactor, and it was found that the gels of examples 2-5 still have flexural properties at-50 c, and the gel of example 1 freezes and hardens at-50 c, rendering the gel inflexible.
In summary, according to the antifreeze moisturizing gel and the preparation method thereof provided by the invention, the antifreeze moisturizing gel is prepared by a solvent replacement method, namely after the hydrogel is prepared, the prepared hydrogel is soaked in the antifreeze moisturizing solvent, and the solvent is exchanged with water in the hydrogel, so that the hydrogel is changed into a mixed system of the solvent with the antifreeze moisturizing effect and the water, and the prepared gel has excellent moisturizing effect and antifreeze performance. The method does not need to control the dosage of the anti-freezing moisturizing solvent, is simple to operate, and can be used for operating various gels.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.

Claims (5)

1. A preparation method of the antifreeze moisturizing gel is characterized by comprising the following steps:
step A, preparing hydrogel;
step B, soaking the prepared hydrogel in an antifreeze moisturizing solvent to replace the antifreeze moisturizing solvent with water in the hydrogel to obtain an antifreeze moisturizing gel; the hydrogel is sodium alginate-acrylamide hydrogel, agar-acrylamide hydrogel, sodium alginate-chitosan hydrogel or PVA-PEG hydrogel; the anti-freezing and moisturizing solvent is glycerol, ethanol, sorbitol, dimethyl sulfoxide/water binary solution or glycol;
the soaking time is 40 min.
2. The method for preparing the antifreeze moisturizing gel as claimed in claim 1, wherein the method for preparing the sodium alginate-acrylamide hydrogel comprises the steps of: dissolving sodium alginate and acrylamide in deionized water, sequentially adding N, N-methylene bisacrylamide and N, N, N ', N' -tetramethyl ethylenediamine, stirring uniformly, and injecting saturated calcium sulfate solution; pouring into a template, and irradiating and molding under ultraviolet light to obtain the sodium alginate-acrylamide hydrogel.
3. The preparation method of the antifreeze moisture-keeping gel as claimed in claim 2, wherein the mass ratio of sodium alginate to acrylamide is (1-3): (5-10).
4. The method for preparing antifreeze moisture-keeping gel according to claim 2, wherein the antifreeze moisture-keeping gel is formed by irradiating under ultraviolet light of 245nm for 40-50 min.
5. An anti-freeze moisturizing gel characterized by being prepared by the preparation method of the anti-freeze moisturizing gel of any one of claims 1 to 4.
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CN109868010A (en) * 2019-01-28 2019-06-11 深圳大学 The method of prepares coating and antifog anti-freeze component on substrate
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