CN110922704A - Preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel - Google Patents
Preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel Download PDFInfo
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- CN110922704A CN110922704A CN201911068578.XA CN201911068578A CN110922704A CN 110922704 A CN110922704 A CN 110922704A CN 201911068578 A CN201911068578 A CN 201911068578A CN 110922704 A CN110922704 A CN 110922704A
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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
- 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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- 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
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—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
- C08J2397/00—Characterised by the use of lignin-containing materials
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Abstract
The invention belongs to the technical field of hydrogel production, and particularly relates to a preparation method of alkali lignin nanoparticle reinforced polyacrylamide hydrogel, which comprises the following steps: preparing 50-70% alkali lignin solution, and placing in a thermostat to keep 30-50 deg.C; preparing 60-75% polyacrylamide solution; mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the step for 1-1.5 h; the hydrophilicity and the biological inertia of Polyacrylamide (PAM) enable the PAM to be widely applied to the field of biological medicine, the polymer molecular chain of the PAM has rich amide groups and can form rich hydrogen bond structures with various groups, alkali lignin is a byproduct of paper making industry, when the alkali lignin and the polyacrylamide act, hydrogel with an interpenetrating network structure can be formed, the hydrogel shows good mechanical properties, biodegradability and the like, and the hydrogel is a multifunctional and environment-friendly product and can enable the alkali lignin to be utilized to achieve win-win effect.
Description
Technical Field
The invention belongs to the technical field of hydrogel production, and particularly relates to preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel.
Background
Hydrogels (hydrogels) are gels that use water as the dispersion medium. The water-soluble polymer with a reticular cross-linked structure is a cross-linked polymer which is formed by introducing a part of hydrophobic groups and hydrophilic residues into the water-soluble polymer, wherein the hydrophilic residues are combined with water molecules to connect the water molecules in the reticular structure, and the hydrophobic residues swell when meeting water. Is a polymer network system, has soft property, can keep a certain shape, and can absorb a large amount of water. All water-soluble or hydrophilic polymers can be subjected to chemical crosslinking or physical crosslinking to form hydrogel. These polymers can be classified into two major categories, natural and synthetic, depending on their origin. The natural hydrophilic polymer includes polysaccharides (starch, cellulose, alginic acid, hyaluronic acid, chitosan, etc.) and polypeptides (collagen, poly-L-lysine, poly-L-glutamic acid, etc.). The synthesized hydrophilic polymer comprises alcohol, acrylic acid and derivatives thereof (polyacrylic acid, polymethacrylic acid, polyacrylamide, poly-N-polyacrylamide and the like).
At present, the synthetic hydrogel needs a plurality of auxiliary materials, and complex synthetic steps and process conditions need to be installed, so that the existing industrial waste cannot be well utilized.
Disclosure of Invention
The invention provides a preparation method of alkali lignin nanoparticle reinforced polyacrylamide hydrogel, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation of alkali lignin nanometer particle reinforced polyacrylamide hydrogel includes the following steps:
s1, preparing 50-70% alkali lignin solution, and placing the solution in a thermostat to keep the temperature at 30-50 ℃;
s2, preparing 60-75% polyacrylamide solution;
s3, mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1-1.5h, standing for 20min, stirring for 20-30min, and standing for 2-3h to obtain the hydrogel.
Preferably, in step S1, the alkali lignin raw material is derived from production waste of a paper mill.
Preferably, the alkali lignin raw material is further purified by acid washing, and is repeatedly washed by deionized water to remove salt after acid washing, dried and purified, added with water and stirred to obtain an alkali lignin solution, and then the alkali lignin solution with the concentration of 50-70% is prepared at the temperature of 30-50 ℃.
Preferably, the polyacrylamide solution is prepared in step S2 by the following method:
s2.1: weighing 1.2-1.5 times of water by weight of polyacrylamide;
s2.2: starting a stirring device, setting the stirring speed to be 250-280 r/min, and simultaneously raising the temperature of the reactor to 55-60 ℃;
s2.3: after the temperature is reached, adding polyacrylamide in corresponding weight parts at the speed of 5g/min, and obtaining 60-75% polyacrylamide solution after the polyacrylamide is completely dissolved.
Preferably, the first stirring temperature in step S3 is 30-40 deg.C, and the first standing temperature is 35-40 deg.C.
Preferably, the second stirring temperature in step S3 is 40-50 deg.C, and the second standing temperature is 40 deg.C.
Compared with the prior art, the invention has the beneficial effects that:
the hydrophilicity and the biological inertia of Polyacrylamide (PAM) enable the PAM to be widely applied to the field of biological medicine, the polymer molecular chain of the PAM has rich amide groups and can form rich hydrogen bond structures with various groups, alkali lignin is a byproduct of paper making industry, when the alkali lignin and the polyacrylamide act, hydrogel with an interpenetrating network structure can be formed, the hydrogel shows good mechanical properties, biodegradability and the like, and the hydrogel is a multifunctional and environment-friendly product and can enable the alkali lignin to be utilized to achieve win-win effect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The invention provides the following technical scheme: the preparation of alkali lignin nanometer particle reinforced polyacrylamide hydrogel includes the following steps:
s1, preparing 50% alkali lignin solution, and placing the solution in a thermostat to keep 30 ℃;
s2, preparing a 60% polyacrylamide solution;
and S3, mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1 hour, standing for 20 minutes, stirring for 20 minutes, and standing for 2 hours to obtain the hydrogel.
In the embodiment, 50% alkali lignin solution is prepared, the alkali lignin raw material is derived from production waste of a paper mill, the alkali lignin raw material is further purified by acid washing, deionized water is used for repeatedly cleaning and desalting after acid washing, water is added for stirring after drying and purification to obtain the alkali lignin solution, and then the 50% alkali lignin solution is prepared at the temperature of 30 ℃ and placed in a thermostat to be kept at the temperature of 30 ℃; preparing 60% polyacrylamide solution, and weighing 1.5 times of water by weight of polyacrylamide; starting a stirring device, setting the stirring speed to be 250r/min, and simultaneously raising the temperature of the reactor to 55 ℃; after the temperature reaches, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and after the polyacrylamide is completely dissolved, obtaining a 60% polyacrylamide solution; mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the above steps for 1 hour, standing for 20 minutes, stirring for 20 minutes again, and standing for 2 hours to obtain the hydrogel, wherein the first stirring temperature is 30 ℃, the first standing temperature is 35 ℃, the second stirring temperature is 40 ℃, and the second standing temperature is 40 ℃.
Specifically, in step S1, the alkali lignin raw material is derived from production waste of a paper mill.
Specifically, the alkali lignin raw material is further purified by acid washing, and is repeatedly washed by deionized water to remove salt after acid washing, dried and purified, added with water and stirred to obtain an alkali lignin solution, and then the alkali lignin solution with the concentration of 50% is prepared at the temperature of 30 ℃.
Specifically, in step S2, the polyacrylamide solution is prepared by the following method:
s2.1: weighing 1.5 times of water by weight of polyacrylamide;
s2.2: starting a stirring device, setting the stirring speed to be 250r/min, and simultaneously raising the temperature of the reactor to 55 ℃;
s2.3: after the temperature is reached, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and obtaining a 60% polyacrylamide solution after the polyacrylamide is completely dissolved.
Specifically, the first stirring temperature in step S3 was 30 ℃ and the first standing temperature was 35 ℃.
Specifically, the second stirring temperature in step S3 was 40 ℃, and the second standing temperature was 40 ℃.
Example 2
The invention provides the following technical scheme: the preparation of alkali lignin nanometer particle reinforced polyacrylamide hydrogel includes the following steps:
s1, preparing 60% alkali lignin solution, and placing the solution in a thermostat to keep the temperature at 40 ℃;
s2, preparing a 68% polyacrylamide solution;
and S3, mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1.2h, standing for 20min, stirring for 25min, and standing for 2.5h to obtain the hydrogel.
In the embodiment, a 60% alkali lignin solution is prepared, the alkali lignin raw material is derived from production waste of a paper mill, the alkali lignin raw material is further purified by acid washing, deionized water is used for repeatedly cleaning and desalting after acid washing, water is added for stirring after drying and purification to obtain the alkali lignin solution, and then the 60% alkali lignin solution is prepared at the temperature of 40 ℃ and placed in a thermostat to be kept at 40 ℃; preparing 68% polyacrylamide solution, and weighing 1.4 times of water by weight of polyacrylamide; starting a stirring device, setting the stirring speed to be 260r/min, and simultaneously raising the temperature of the reactor to 58 ℃; after the temperature reaches, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and obtaining a 68% polyacrylamide solution after the polyacrylamide is completely dissolved; mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1.2h, standing for 20min, stirring for 25min, and standing for 2.5h to obtain the hydrogel, wherein the first stirring temperature is 35 ℃, the first standing temperature is 38 ℃, the second stirring temperature is 45 ℃, and the second standing temperature is 40 ℃.
Specifically, in step S1, the alkali lignin raw material is derived from production waste of a paper mill.
Specifically, the alkali lignin raw material is further purified by acid washing, and is repeatedly washed by deionized water to remove salt after acid washing, dried and purified, added with water and stirred to obtain an alkali lignin solution, and then the alkali lignin solution with the concentration of 60% is prepared at the temperature of 40 ℃.
Specifically, in step S2, the polyacrylamide solution is prepared by the following method:
s2.1: weighing 1.4 times of water by weight of polyacrylamide;
s2.2: starting a stirring device, setting the stirring speed to be 260r/min, and simultaneously raising the temperature of the reactor to 58 ℃;
s2.3: after the temperature is reached, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and obtaining a 68% polyacrylamide solution after the polyacrylamide is completely dissolved.
Specifically, the first stirring temperature in step S3 was 35 ℃, and the first standing temperature was 38 ℃.
Specifically, the second stirring temperature in step S3 was 45 ℃ and the second standing temperature was 40 ℃.
Example 3
The invention provides the following technical scheme: the preparation of alkali lignin nanometer particle reinforced polyacrylamide hydrogel includes the following steps:
s1, preparing 70% alkali lignin solution, and placing the solution in a thermostat to keep 50 ℃;
s2, preparing a 75% polyacrylamide solution;
and S3, mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1.5 hours, standing for 20 minutes, stirring for 30 minutes, and standing for 3 hours to obtain the hydrogel.
In the embodiment, 70% alkali lignin solution is prepared, the alkali lignin raw material is derived from production waste of a paper mill, the alkali lignin raw material is further purified by acid washing, deionized water is used for repeatedly cleaning and desalting after acid washing, water is added for stirring after drying and purification to obtain the alkali lignin solution, and then the 70% alkali lignin solution is prepared at the temperature of 50 ℃ and placed in a thermostat to be kept at 50 ℃; preparing 75% polyacrylamide solution, and weighing 1.2 times of water by weight of polyacrylamide; starting a stirring device, setting the stirring speed to be 280r/min, and simultaneously raising the temperature of the reactor to 60 ℃; after the temperature reaches, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and obtaining 75% polyacrylamide solution after the polyacrylamide is completely dissolved; mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1.5h, standing for 20min, stirring for 30min, and standing for 3h to obtain the hydrogel, wherein the first stirring temperature is 40 ℃, the first standing temperature is 40 ℃, the second stirring temperature is 50 ℃, and the second standing temperature is 40 ℃.
Specifically, in step S1, the alkali lignin raw material is derived from production waste of a paper mill.
Specifically, the alkali lignin raw material is further purified by acid washing, and is repeatedly washed by deionized water to remove salt after acid washing, dried and purified, added with water and stirred to obtain an alkali lignin solution, and then the alkali lignin solution with the concentration of 70% is prepared at the temperature of 50 ℃.
Specifically, in step S2, the polyacrylamide solution is prepared by the following method:
s2.1: weighing 1.2 times of water by weight of polyacrylamide;
s2.2: starting a stirring device, setting the stirring speed to be 280r/min, and simultaneously raising the temperature of the reactor to 60 ℃;
s2.3: after the temperature is reached, adding polyacrylamide in a corresponding weight part at the speed of 5g/min, and obtaining 75% polyacrylamide solution after the polyacrylamide is completely dissolved.
Specifically, the first stirring temperature in step S3 was 40 ℃, and the first standing temperature was 40 ℃.
Specifically, the second stirring temperature in step S3 was 50 ℃ and the second standing temperature was 40 ℃.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification made within the spirit and principles of the present invention.
Claims (6)
1. The preparation method of the alkali lignin nanoparticle reinforced polyacrylamide hydrogel is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing 50-70% alkali lignin solution, and placing the solution in a thermostat to keep the temperature at 30-50 ℃;
s2, preparing 60-75% polyacrylamide solution;
s3, mixing and stirring the polyacrylamide solution and the alkali lignin solution prepared in the steps for 1-1.5h, standing for 20min, stirring for 20-30min, and standing for 2-3h to obtain the hydrogel.
2. The preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel according to claim 1, wherein the alkali lignin nanoparticle reinforced polyacrylamide hydrogel comprises: in step S1, the alkali lignin feedstock is derived from production waste from a paper mill.
3. The preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel according to claim 2, wherein the alkali lignin nanoparticle reinforced polyacrylamide hydrogel comprises: further purifying the alkali lignin raw material by acid washing, repeatedly cleaning and desalting with deionized water after acid washing, drying and purifying, adding water and stirring to obtain an alkali lignin solution, and then preparing the 50-70% alkali lignin solution at the temperature of 30-50 ℃.
4. The preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel according to claim 1, wherein the alkali lignin nanoparticle reinforced polyacrylamide hydrogel comprises: the polyacrylamide solution is prepared in step S2 by the following method:
s2.1: weighing 1.2-1.5 times of water by weight of polyacrylamide;
s2.2: starting a stirring device, setting the stirring speed to be 250-280 r/min, and simultaneously raising the temperature of the reactor to 55-60 ℃;
s2.3: after the temperature is reached, adding polyacrylamide in corresponding weight parts at the speed of 5g/min, and obtaining 60-75% polyacrylamide solution after the polyacrylamide is completely dissolved.
5. The preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel according to claim 1, wherein the alkali lignin nanoparticle reinforced polyacrylamide hydrogel comprises: the first stirring temperature in step S3 is 30-40 deg.C, and the first standing temperature is 35-40 deg.C.
6. The preparation of alkali lignin nanoparticle reinforced polyacrylamide hydrogel according to claim 1, wherein the alkali lignin nanoparticle reinforced polyacrylamide hydrogel comprises: the second stirring temperature in step S3 was 40-50 ℃ and the second standing temperature was 40 ℃.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111732807A (en) * | 2020-07-06 | 2020-10-02 | 安徽农业大学 | Lignin composite polyamide self-healing material and preparation method thereof |
CN112661981A (en) * | 2020-12-11 | 2021-04-16 | 齐鲁工业大学 | Multifunctional hydrogel triggered by lignin phenolic resin silver-loaded nanospheres and preparation method and application thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111732807A (en) * | 2020-07-06 | 2020-10-02 | 安徽农业大学 | Lignin composite polyamide self-healing material and preparation method thereof |
CN112661981A (en) * | 2020-12-11 | 2021-04-16 | 齐鲁工业大学 | Multifunctional hydrogel triggered by lignin phenolic resin silver-loaded nanospheres and preparation method and application thereof |
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Application publication date: 20200327 |