CN112940289A - Preparation method of high-performance hydrogel - Google Patents
Preparation method of high-performance hydrogel Download PDFInfo
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- CN112940289A CN112940289A CN202110154778.8A CN202110154778A CN112940289A CN 112940289 A CN112940289 A CN 112940289A CN 202110154778 A CN202110154778 A CN 202110154778A CN 112940289 A CN112940289 A CN 112940289A
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/24—Homopolymers or copolymers of amides or imides
- C08J2433/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The invention discloses a preparation method of high-performance hydrogel, which comprises the following steps of 1) carrying out surface treatment on porous silicon rubber to enable the surface of the porous silicon rubber to be provided with polar groups; 2) reacting a silane coupling agent or a polyfunctional epoxy compound with a polar group on the surface of the porous silicon rubber, and grafting a reactive group; 3) and uniformly mixing the water solution of the water-soluble monomer, the initiator, the cross-linking agent, the water-soluble polymer and the inorganic salt, adding the mixture into the porous silicon rubber treated in the step 2), and heating and reacting for a period of time to obtain the high-performance hydrogel. The hydrogel provided by the invention has high elasticity and high toughness of the silicon rubber, so that the hydrogel has higher mechanical properties; the aperture of the porous silicon rubber is micron scale, and the porous silicon rubber can be combined with the monomer of the hydrogel through a covalent bond through surface treatment, so that the compatibility is good; the introduced water-soluble polymer and the multivalent inorganic salt can be biologically crosslinked and form an interpenetrating network structure with the hydrogel formed by polymerization, so that the physical properties of the hydrogel are improved.
Description
Technical Field
The invention relates to a preparation method of hydrogel, in particular to a preparation method of high-performance hydrogel.
Background
The hydrogel is a multi-component system composed of three-dimensional cross-linked network structure high polymer and medium, and has excellent properties of good water absorption, water retention, biocompatibility, corresponding intelligent property to stimulation and the like, so that the application of the hydrogel has been penetrated into the fields of agriculture, forestry, pasture, horticulture, desert control, medical treatment and health, biomedicine, construction, petrochemical industry, daily chemical industry, food, electronics, environmental protection and the like, and still expands to wider application fields.
However, most of the hydrogels made from natural or synthetic materials have poor mechanical properties. Hydrogels of conventional construction tend to have certain mechanical properties at relatively low water contents, while at higher water contents (e.g., > 90% by mass) the mechanical strength is significantly reduced, and even fracture occurs at very low pressures, limiting their practical utility.
Therefore, from the aspect of enhancing the mechanical strength of the hydrogel, the preparation of the composite gel material with good compression resistance and high mechanical strength by compounding a plurality of components becomes a research hotspot.
Disclosure of Invention
Aiming at the defects of the prior art, the invention compounds the porous silicon rubber and the hydrogel and provides a preparation method of the high-performance hydrogel.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of high-performance hydrogel is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1), providing porous silicon rubber, and carrying out surface treatment on the porous silicon rubber to enable the surface of the porous silicon rubber to be provided with polar groups, wherein the polar groups are any one or more of hydroxyl, carbonyl, aldehyde and carboxyl;
step 2), coating a silane coupling agent or a polyfunctional epoxy compound on the surface of the porous silicon rubber treated in the step 1), so that the silane coupling agent or the polyfunctional epoxy compound reacts with polar groups on the surface of the porous silicon rubber, and grafting reactive groups on the surface of the porous silicon rubber; the reaction temperature is 20-150 ℃, and the reaction time is 1-60 minutes;
and 3) uniformly mixing the water solution of the water-soluble monomer, the initiator, the cross-linking agent, the water-soluble polymer and the inorganic salt, adding the mixture into the porous silicon rubber treated in the step 2), and heating and reacting for a period of time to obtain the high-performance hydrogel.
Further, the preparation method of the porous silicone rubber comprises the following steps: 1) uniformly mixing 100 parts of vinyl-containing polysiloxane, 5-30 parts of organohydrogenpolysiloxane, 0.01-1 part of hydrosilylation catalyst, 20-500 parts of water-containing super absorbent resin and 0.1-5 parts of silicone oil surfactant; 2) heating and curing the mixture obtained in the step 1) at 50-200 ℃ to obtain silicon rubber; 3) drying and dewatering the silicone rubber obtained in the step 2) to obtain the porous silicone rubber.
Still further, the vinyl-containing polysiloxane is a polydiorganosiloxane containing two or more vinyl groups; the organic hydrogen polysiloxane is organic hydrogen polysiloxane containing three or more Si-H; the super absorbent resin is polyacrylic acid and salt thereof, and polyacrylamide cross-linked network polymer; the hydrosilylation catalyst is a platinum metal complex catalyst; the silicone oil surfactant is a polyorganosiloxane-polyoxyethylene copolymer.
Further, in the step 1), the surface treatment method is an ultraviolet light irradiation treatment method or a plasma surface treatment method; the wavelength of the ultraviolet light in the ultraviolet light irradiation treatment method is 170-260 nm, and the time is 1-120 minutes.
Further, the silane coupling agent comprises at least one of 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane; the multifunctional epoxy compound comprises at least one of trimethylolpropane triglycidyl ether, trimethylolethane triglycidyl ether, polyglycerol triglycidyl ether, propoxyglycerol triglycidyl ether, glycerol triglycidyl ether, tetraglycidyl ether tetraphenylethane, triglycidyl ether triphenylmethane and tetraglycidyl diaminodiphenylmethane.
Further, the water-soluble monomer is at least one of acrylic acid and salts thereof, methacrylic acid and salts thereof, acrylamide, methacrylamide, acrylic sulfonate and methacrylic sulfonate.
Further, the initiator is azo water-soluble initiator, persulfate initiator and peroxide initiator; the azo water-soluble initiator comprises any one of azodiisobutyl amidine hydrochloride, azodiisobutyl imidazoline hydrochloride, azodicyano valeric acid and azodiisopropyl imidazoline; the persulfate initiator comprises any one of potassium persulfate, sodium persulfate and ammonium persulfate; the peroxide initiator comprises any one of hydrogen peroxide, tert-butyl peroxide and methyl ethyl ketone peroxide; the initiator also comprises a persulfate initiator, a peroxide initiator and a reducing agent to form an oxidation-reduction system; the reducing agent comprises any one of L-ascorbic acid, sulfite, bisulfite and ferrous salt; the amount of the initiator is 0.0001 to 1 mol% based on the water-soluble monomer.
Further, the cross-linking agent is at least one of ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, ethylene glycol diacrylate, polyethylene glycol diacrylate and N, N-methylene bisacrylamide.
Further, the water-soluble polymer is sodium alginate.
Further, the inorganic salt is a polyvalent metal salt; the polyvalent metal salt includes calcium chloride, magnesium chloride, ferric sulfate, and aluminum sulfate.
The invention has the beneficial effects that: compared with the prior art, the high-performance hydrogel provided by the invention has the following advantages:
1) compounding silicon rubber and hydrogel to make the hydrogel have high elasticity and high toughness of the silicon rubber, thereby endowing the hydrogel with higher mechanical property;
2) the adopted silicone rubber is porous silicone rubber, the pore diameter is micron scale, and the surface is processed, so that the silicone rubber can react with the monomer of the hydrogel, the hydrogel is combined with the silicone rubber through a covalent bond, and the compatibility is good;
3) the introduced water-soluble polymer and the multivalent inorganic salt can be physically crosslinked and form an interpenetrating network structure with the hydrogel formed by polymerization, so that the physical properties of the hydrogel are further improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
(1) Preparation of porous silicon rubber
100 parts by mass of a vinyl-containing polysiloxane having a viscosity of 740 pas at 25 ℃, 20 parts by mass of an organohydrogenpolysiloxane having a viscosity of 0.5 mPas at 25 ℃, 0.12 part of a platinum catalyst having a platinum content of 1000ppm, 20 parts of a water-containing super absorbent resin (average particle diameter 10 μm, water absorption capacity 50 times), 0.1 part of a silicone oil surfactant and 10 parts of fumed silica were mixed under vacuum, and the mixture was cured by heating to obtain a silicone rubber composition. Drying at 100 ℃ for 20 hours to obtain the porous silicon rubber.
(2) High performance hydrogel preparation
Step 1), irradiating the prepared porous silicon rubber for 60 minutes under ultraviolet light with the wavelength of 170 nm-260 nm;
step 2), spraying a silane coupling agent gamma-glycidoxypropyltrimethoxysilane on the surface of the porous silicon rubber treated in the step 1), and reacting for 30 minutes at 100 ℃;
and 3) uniformly mixing 100 parts of acrylic acid, 0.2 part of initiator potassium persulfate, 300 parts of water, 0.1 part of cross-linking agent polyethylene glycol diacrylate, 2 parts of sodium alginate and 0.001 part of calcium chloride, adding the mixture into the porous silicon rubber treated in the step 2), and heating the mixture at 70 ℃ for reacting for 60 minutes to obtain the high-performance hydrogel.
Example 2
(1) Preparation of porous silicon rubber
100 parts by mass of a vinyl-containing polysiloxane having a viscosity of 740 pas at 25 ℃, 20 parts by mass of an organohydrogenpolysiloxane having a viscosity of 0.5 mPas at 25 ℃, 0.12 part of a platinum catalyst having a platinum content of 1000ppm, 20 parts of a water-containing super absorbent resin (average particle diameter 10 μm, water absorption capacity 50 times), 0.1 part of a silicone oil surfactant and 10 parts of fumed silica were mixed under vacuum, and the mixture was cured by heating to obtain a silicone rubber composition. Drying at 100 ℃ for 20 hours to obtain the porous silicon rubber.
(2) High performance hydrogel preparation
Step 1), treating the prepared porous silicon rubber for 5 minutes under plasma;
step 2), spraying a silane coupling agent gamma- (methacryloyloxy) propyl trimethoxy silane on the surface of the porous silicon rubber treated in the step 1), and reacting for 30 minutes at 80 ℃;
and 3) uniformly mixing 100 parts of acrylic acid, 0.2 part of initiator potassium persulfate, 300 parts of water, 0.1 part of cross-linking agent ethylene glycol diacrylate, 2 parts of sodium alginate and 0.002 part of calcium chloride, adding the mixture into the porous silicon rubber treated in the step 2), and heating the mixture at 70 ℃ for reacting for 60 minutes to obtain the high-performance hydrogel.
Example 3
(1) Preparation of porous silicon rubber
100 parts by mass of a vinyl-containing polysiloxane having a viscosity of 740 pas at 25 ℃, 20 parts by mass of an organohydrogenpolysiloxane having a viscosity of 0.5 mPas at 25 ℃, 0.12 part of a platinum catalyst having a platinum content of 1000ppm, 20 parts of a water-containing super absorbent resin (average particle diameter 10 μm, water absorption capacity 50 times), 0.1 part of a silicone oil surfactant and 10 parts of fumed silica were mixed under vacuum, and the mixture was cured by heating to obtain a silicone rubber composition. Drying at 100 ℃ for 20 hours to obtain the porous silicon rubber.
(2) High performance hydrogel preparation
Step 1), irradiating the prepared porous silicon rubber for 60 minutes under ultraviolet light with the wavelength of 170 nm-260 nm;
step 2), spraying a silane coupling agent gamma- (methacryloyloxy) propyl trimethoxy silane on the surface of the porous silicon rubber treated in the step 1), and reacting for 30 minutes at 80 ℃;
and 3) uniformly mixing 100 parts of acrylic acid, 10 parts of acrylamide, 0.3 part of initiator potassium persulfate, 250 parts of water, 0.1 part of cross-linking agent ethylene glycol diacrylate, 2 parts of sodium alginate and 0.002 part of calcium chloride, adding the mixture into the porous silicon rubber treated in the step 2), and heating the mixture to 70 ℃ for reaction for 60 minutes to obtain the high-performance hydrogel.
Comparative example 1
100 parts of acrylic acid, 0.2 part of initiator potassium persulfate, 300 parts of water, 0.1 part of cross-linking agent ethylene glycol diacrylate, 2 parts of sodium alginate and 0.002 part of calcium chloride are uniformly mixed, and the mixture is heated at 70 ℃ to react for 60 minutes, so that the high-performance hydrogel can be obtained.
TABLE 1
| Elongation at Break (%) | Tensile Strength (MPa) | |
| Example 1 | 950 | 2.3 |
| Example 2 | 832 | 1.98 |
| Example 3 | 905 | 2.1 |
| Comparative example 1 | 330 | 1.45 |
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (10)
1. A preparation method of high-performance hydrogel is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1), providing porous silicon rubber, and carrying out surface treatment on the porous silicon rubber to enable the surface of the porous silicon rubber to be provided with polar groups, wherein the polar groups are any one or more of hydroxyl, carbonyl, aldehyde and carboxyl;
step 2), coating a silane coupling agent or a polyfunctional epoxy compound on the surface of the porous silicon rubber treated in the step 1), so that the silane coupling agent or the polyfunctional epoxy compound reacts with polar groups on the surface of the porous silicon rubber, and grafting reactive groups on the surface of the porous silicon rubber; the reaction temperature is 20-150 ℃, and the reaction time is 1-60 minutes;
and 3) uniformly mixing the water solution of the water-soluble monomer, the initiator, the cross-linking agent, the water-soluble polymer and the inorganic salt, adding the mixture into the porous silicon rubber treated in the step 2), and heating and reacting for a period of time to obtain the high-performance hydrogel.
2. The method of claim 1, wherein the hydrogel comprises: the preparation method of the porous silicon rubber comprises the following steps: 1) uniformly mixing 100 parts of vinyl-containing polysiloxane, 5-30 parts of organohydrogenpolysiloxane, 0.01-1 part of hydrosilylation catalyst, 20-500 parts of water-containing super absorbent resin and 0.1-5 parts of silicone oil surfactant; 2) heating and curing the mixture obtained in the step 1) at 50-200 ℃ to obtain silicon rubber; 3) drying and dewatering the silicone rubber obtained in the step 2) to obtain the porous silicone rubber.
3. The method of claim 2, wherein the hydrogel comprises: the vinyl-containing polysiloxane is polydiorganosiloxane containing two or more vinyl groups; the organic hydrogen polysiloxane is organic hydrogen polysiloxane containing three or more Si-H; the super absorbent resin is polyacrylic acid and salt thereof, and polyacrylamide cross-linked network polymer; the hydrosilylation catalyst is a platinum metal complex catalyst; the silicone oil surfactant is a polyorganosiloxane-polyoxyethylene copolymer.
4. The method of claim 1, wherein the hydrogel comprises: in the step 1), the surface treatment method is an ultraviolet light irradiation treatment method or a plasma surface treatment method; the wavelength of the ultraviolet light in the ultraviolet light irradiation treatment method is 170-260 nm, and the time is 1-120 minutes.
5. The method of claim 1, wherein the hydrogel comprises: the silane coupling agent comprises at least one of 3-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane; the multifunctional epoxy compound comprises at least one of trimethylolpropane triglycidyl ether, trimethylolethane triglycidyl ether, polyglycerol triglycidyl ether, propoxyglycerol triglycidyl ether, glycerol triglycidyl ether, tetraglycidyl ether tetraphenylethane, triglycidyl ether triphenylmethane and tetraglycidyl diaminodiphenylmethane.
6. The method of claim 1, wherein the hydrogel comprises: the water-soluble monomer is at least one of acrylic acid and salts thereof, methacrylic acid and salts thereof, acrylamide, methacrylamide, acrylic sulfonate and methacrylic sulfonate.
7. The method of claim 1, wherein the hydrogel comprises: the initiator is azo water-soluble initiator, persulfate initiator and peroxide initiator; the azo water-soluble initiator comprises any one of azodiisobutyl amidine hydrochloride, azodiisobutyl imidazoline hydrochloride, azodicyano valeric acid and azodiisopropyl imidazoline; the persulfate initiator comprises any one of potassium persulfate, sodium persulfate and ammonium persulfate; the peroxide initiator comprises any one of hydrogen peroxide, tert-butyl peroxide and methyl ethyl ketone peroxide; the initiator also comprises a persulfate initiator, a peroxide initiator and a reducing agent to form an oxidation-reduction system; the reducing agent comprises any one of L-ascorbic acid, sulfite, bisulfite and ferrous salt; the amount of the initiator is 0.0001 to 1 mol% based on the water-soluble monomer.
8. The method of claim 1, wherein the hydrogel comprises: the cross-linking agent is at least one of ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, ethylene glycol diacrylate, polyethylene glycol diacrylate and N, N-methylene bisacrylamide.
9. The method of claim 1, wherein the hydrogel comprises: the water-soluble polymer is sodium alginate.
10. The method of claim 1, wherein the hydrogel comprises: the inorganic salt is a multivalent metal salt; the polyvalent metal salt includes calcium chloride, magnesium chloride, ferric sulfate, and aluminum sulfate.
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| CN114290783A (en) * | 2021-11-24 | 2022-04-08 | 四川师范大学 | Antibacterial moisturizing double-layer material and preparation method thereof |
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| CN114290783A (en) * | 2021-11-24 | 2022-04-08 | 四川师范大学 | Antibacterial moisturizing double-layer material and preparation method thereof |
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Application publication date: 20210611 |