CN109897197A - A kind of sodium lignin sulfonate aquagel and preparation method thereof - Google Patents
A kind of sodium lignin sulfonate aquagel and preparation method thereof Download PDFInfo
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- CN109897197A CN109897197A CN201910185727.4A CN201910185727A CN109897197A CN 109897197 A CN109897197 A CN 109897197A CN 201910185727 A CN201910185727 A CN 201910185727A CN 109897197 A CN109897197 A CN 109897197A
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Abstract
The invention discloses a kind of sodium lignin sulfonate aquagel and preparation method thereof, 1) sodium lignin sulfonate, chitosan and vinyl polymerization monomer are weighed, it is dissolved in deionized water；2) water-soluble cellulose ether is added in Xiang Shangshu solution, is dissolved in weakly acidic solution, and be uniformly mixed, form the solution of stable homogeneous；3) crosslinking agent, initiator then are added to step 2 acquired solution, stirring is to being completely dissolved；4) in the environment of the mixed solution of step 3 being then placed in 35-40 DEG C, heating water bath is carried out, Raolical polymerizable is complete, and required hydrogel can be prepared；5) surface is cleaned multiple times with distilled water in hydrogel made from step 4, removes the unreacted impurity in surface.With sodium lignin sulfonate, chitosan etc., for raw material, the product is prepared by simple, easily-controllable Raolical polymerizable in situ in the present invention, has excellent mechanical performance and swelling behavior, and can effectively be adsorbed to organic dye molecule.
Description
Technical field
The present invention relates to new bio technical field of polymer materials, in particular to a kind of sodium lignin sulfonate chitosan water
Gel and preparation method thereof.
Background technique
Macromolecule hydrogel is one kind using water as decentralized medium, the high molecular polymerization with three-dimensional crosslinked network structure
Object can be absorbed a large amount of moisture and be swollen, and reaches and be still able to maintain its original structure after swelling equilibrium and be not destroyed.Together
When hydrogel also there is hydrophilic three-dimensional net structure, can be absorbed a large amount of pollutant, and by carboxyl, amide groups, hydroxyl,
The groups such as sulfonic group adsorb contents of many kinds of heavy metal ion and pigment molecular, to achieve the effect that decontaminate water purification.In addition, it also has
Good biocompatibility, in organizational project, pharmaceutical carrier, contact lenses, before sewage treatment etc. has a wide range of applications
Scape.But traditional hydrogel limits its reality in life and answers because mechanical performance is poor and adsorption efficiency is not high
With so the widely used hydrogel of the energy of synthesizing new is the problem of primarily now research.
At present in research, the preparation of most of high intensity hydrogel and is naturally gathered using synthetic polymer as raw material
Object is closed but to be rarely used.Lignin is deputy most abundant natural reproducible resource in the world, by lilac base propane,
Three kinds of basic units of guaiacyl propane and para hydroxybenzene propane are constituted, and contain various active functional group in molecular structure,
How the probing direction that higher value application is also present researcher is carried out to it.
Chitosan is a kind of presently found unique trona, is to pass through Isosorbide-5-Nitrae sugar by 2- amino -2-DG
The positively charged straight-chain polysaccharide of glycosidic bond connection.Many hydroxyls, amino and N- acetylamino etc. are dispersed in chitosan molecule chain
Group, these groups can form intermolecular and intramolecular hydrogen bond between each other so that its be difficult in organic solvent, water and alkali it is molten
Solution.But in dilute acid soln, since protonated amino destroys the hydrogen bond action of intramolecular, to keep chitosan effectively molten
Solution.In addition, chitosan has from a wealth of sources, cheap and easy to get, good biocompatibility, biological degradability and natural antibacterial
The characteristics such as property, nontoxicity, are the ideal materials for preparing hydrogel.There is very strong moisture absorption, moisturizing as the hydrogel prepared by it
Performance together and can also enhance certain adsorptivity, so that it can be widely applied to the fields such as medicine, industry.
It is an object of the invention to realize to make full use of lignin and chitosan, while improving the machinery of hydrogel
Performance, toughness, moisture absorbability and moisture retentivity and absorption property.It is described with sodium lignin sulfonate, chitosan, acrylic acid, N, N '-methylene
Base bisacrylamide and hydrogen peroxide etc. are raw material sodium lignin sulfonate chitosan water-setting as made from Raolical polymerizable
Glue, presents higher toughness, intensity, that is, is demonstrated by good mechanical performance, at the same the hydrogel have in water it is higher
Swelling ratio and excellent adsorption rate can be used as absorption organic dyestuff or heavy metal ion.In addition, hydrogel is prepared
Preparation method simple process, low in raw material price, preparation process is environmental-friendly pollution-free, product can natural degradation, can be further
Large-scale promotion application.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the above technological deficiencies, solve conventional hydrogels mechanical performance and absorption
The disadvantages of performance is poor, while environment is protected, propose a kind of degradable, reproducible sodium lignin sulfonate aquagel
And preparation method thereof.
In order to achieve the above object of the invention, the technical solution adopted by the present invention are as follows:
A kind of sodium lignin sulfonate aquagel and preparation method thereof, comprising the following steps:
1) sodium lignin sulfonate, chitosan and vinyl polymerization monomer are weighed, is dissolved in deionized water, solution is obtained；
2) water-soluble cellulose ether is added in Xiang Shangshu solution, is dissolved in weakly acidic solution, and be uniformly mixed, formed
The solution of stable homogeneous；
3) crosslinking agent, initiator then are added to step 2 acquired solution, stirring is uniformly mixed to being completely dissolved；
4) in the environment of the mixed solution of step 3 being then placed in 35-40 DEG C, heating water bath, free radical polymerization are carried out
Required hydrogel can be prepared in fully reacting；
5) surface is cleaned multiple times with distilled water in hydrogel made from step 4, removes the unreacted impurity in surface.
Further, the vinyl polymerization monomer includes in acrylic acid, acrylamide, vinyl alcohol and vinyl pyrrolidone
One or several kinds of mixtures.
Further, the crosslinking agent includes N, N '-methylene-bisacrylamide, ethylene glycol dimethacrylate, two
One or several kinds of mixture in vinyl benzene and diisocyanate.
Further, the initiator include it is a kind of in hydrogen peroxide, ascorbic acid, potassium peroxydisulfate and ammonium persulfate or
Several mixtures.
A kind of sodium lignin sulfonate aquagel is made by the described in any item preparation methods of claim 1-4.
Further, lignin sulfonic acid sodium content accounts for the 5-30% of overall solid content in the hydrogel of preparation.
Further, chitosan content accounts for the 8-10% of overall solid content in the hydrogel of preparation.
Further, content of crosslinking agent accounts for the 0.5-1% of overall solid content in the hydrogel of preparation.
Further, the content of polymer accounts for the 65-95% of overall solid content in the hydrogel of preparation.
The invention has the benefit that the present invention with sodium lignin sulfonate, chitosan etc. for raw material, by simple, easily-controllable
Raolical polymerizable in situ the product is prepared, it is with excellent mechanical performance and swelling behavior as the result is shown, and
Organic dye molecule can effectively be adsorbed；
1. one of primary raw material disclosed by the invention for preparing hydrogel is the wood extracted in pulping and paper-making waste liquid
Quality sodium sulfonate, is successfully realized waste utilization；
2. one of primary raw material disclosed by the invention for preparing hydrogel is chitosan, from a wealth of sources, obtains and be easy, it is raw
Produce it is low in cost, and have good biocompatibility, biological degradability and natural antibiotic property；
3. the hydrogel being prepared using method disclosed by the invention have excellent mechanical performance and swelling behavior with
And good Dye Adsorption performance, biocompatibility and advantages of environment protection；
4. the preparation method using sodium lignin sulfonate aquagel disclosed by the invention is simple, short preparation period,
Production cost is low, can be promoted the use of on a large scale.
Specific embodiment
In order that the present invention can be more clearly and readily understood, below technical solution in the embodiment of the present invention into
Row clearly and completely describes.
Embodiment one:
The acrylic acid of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g hydroxyethyl cellulose is added into above-mentioned solution again, is dissolved in
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；The N that 0.3-0.5g is added is then continued to, N '-is sub-
For bisacrylamide as crosslinking agent, 400-600 μ l concentration is the ascorbic acid solution of 0.5-1.5% as initiator, is mixed
It closes uniform；Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is finally placed in 35-40 DEG C.Reaction knot
Hydrogel surface is cleaned multiple times with distilled water to remove the unreacted impurity in surface in Shu Hou.
Embodiment two:
The acrylamide for weighing the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g, by it
It is dissolved in 20-30ml deionized water, is allowed to be completely dissolved；2-4g hydroxyethyl cellulose is added into above-mentioned solution again, its is molten
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；Then continue to N, N '-that 0.3-0.5g is added
For methylene-bisacrylamide as crosslinking agent, 400-600 μ l concentration is the hydrogen peroxide of 3-6% as initiator, is uniformly mixed；Most
Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is placed in 35-40 DEG C afterwards.After reaction, with steaming
Hydrogel surface is cleaned multiple times to remove the unreacted impurity in surface in distilled water.
Embodiment three:
The vinyl alcohol of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g hydroxyethyl cellulose is added into above-mentioned solution again, is dissolved in
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；The N that 0.3-0.5g is added is then continued to, N '-is sub-
For bisacrylamide as crosslinking agent, 400-600 μ l concentration is the ascorbic acid solution of 0.5-1.5% as initiator, is mixed
It closes uniform；Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is finally placed in 35-40 DEG C.Reaction knot
Hydrogel surface is cleaned multiple times with distilled water to remove the unreacted impurity in surface in Shu Hou.
Example IV:
The acrylic acid of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g hydroxypropyl cellulose is added into above-mentioned solution again, is dissolved in
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；The N that 0.3-0.5g is added is then continued to, N '-is sub-
For bisacrylamide as crosslinking agent, 400-600 μ l concentration is the hydrogen peroxide of 3-6% as initiator, is uniformly mixed；Finally
Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is placed in 35-40 DEG C.After reaction, with distillation
Hydrogel surface is cleaned multiple times to remove the unreacted impurity in surface in water.
Embodiment five:
The acrylic acid of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g methylcellulose is added into above-mentioned solution again, is dissolved in weak
It in acid solution, and is uniformly mixed, forms the solution of stable homogeneous；Then continue to the N that 0.3-0.5g is added, N '-methylene
For base bisacrylamide as crosslinking agent, 400-600 μ l concentration is the ascorbic acid solution of 0.5-1.5% as initiator, mixing
Uniformly；Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is finally placed in 35-40 DEG C.Reaction terminates
Afterwards, hydrogel surface is cleaned multiple times with distilled water to remove the unreacted impurity in surface.
Embodiment six:
The acrylic acid of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g ethyl cellulose is added into above-mentioned solution again, is dissolved in weak
It in acid solution, and is uniformly mixed, forms the solution of stable homogeneous；Then continue to the N that 0.3-0.5g is added, N '-methylene
For base bisacrylamide as crosslinking agent, 400-600 μ l concentration is the hydrogen peroxide of 3-6% as initiator, is uniformly mixed；Finally will
Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is placed in 35-40 DEG C.After reaction, distilled water is used
Hydrogel surface is cleaned multiple times to remove the unreacted impurity in surface.
Embodiment seven:
The acrylic acid of the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g is weighed, its is molten
In 20-30ml deionized water, it is allowed to be completely dissolved；2-4g hydroxypropyl methyl cellulose is added into above-mentioned solution again, by it
It is dissolved in weakly acidic solution, and is uniformly mixed, form the solution of stable homogeneous；The N that 0.3-0.5g is added is then continued to,
For N '-methylene-bisacrylamide as crosslinking agent, 400-600 μ l concentration is the ascorbic acid solution of 0.5-1.5% as initiation
Agent is uniformly mixed；Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is finally placed in 35-40 DEG C.
After reaction, hydrogel surface is cleaned multiple times with distilled water to remove the unreacted impurity in surface.
Embodiment eight:
The acrylamide for weighing the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g, by it
It is dissolved in 20-30ml deionized water, is allowed to be completely dissolved；2-4g hydroxymethyl cellulose is added into above-mentioned solution again, its is molten
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；Then continue to N, N '-that 0.3-0.5g is added
For methylene-bisacrylamide as crosslinking agent, 400-600 μ l concentration is the hydrogen peroxide of 3-6% as initiator, is uniformly mixed；Most
Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is placed in 35-40 DEG C afterwards.After reaction, with steaming
Hydrogel surface is cleaned multiple times to remove the unreacted impurity in surface in distilled water.
Embodiment nine:
The acrylamide for weighing the sodium lignin sulfonate of 1.0-1.5g, the chitosan of 1.2-1.8g and 0.3-0.5g, by it
It is dissolved in 20-30ml deionized water, is allowed to be completely dissolved；2-4g hydroxyethyl cellulose is added into above-mentioned solution again, its is molten
It in weakly acidic solution, and is uniformly mixed, forms the solution of stable homogeneous；Then continue to the dimethyl that 0.3-0.5g is added
For acrylic acid glycol ester as crosslinking agent, 400-600 μ l concentration is the ascorbic acid solution of 0.5-1.5% as initiator, is mixed
It closes uniform；Required hydrogel can be obtained in reaction 20-30h in the environment of this reaction is finally placed in 35-40 DEG C.Reaction knot
Hydrogel surface is cleaned multiple times with distilled water to remove the unreacted impurity in surface in Shu Hou.
The present invention and its embodiments have been described above, this description is no restricted, only reality of the invention
One of mode is applied, actual embodiment is not limited thereto.All in all if those skilled in the art are opened by it
Show, without departing from the spirit of the invention, not inventively design embodiment similar with the technical solution,
It is within the scope of protection of the invention.
Claims (9)
1. a kind of sodium lignin sulfonate aquagel and preparation method thereof, it is characterised in that: the following steps are included:
1) sodium lignin sulfonate, chitosan and vinyl polymerization monomer are weighed, is dissolved in deionized water, solution is obtained；
2) water-soluble cellulose ether is added in Xiang Shangshu solution, is dissolved in weakly acidic solution, and be uniformly mixed, formed uniform
Stable solution；
3) crosslinking agent, initiator then are added to step 2 acquired solution, stirring is uniformly mixed to being completely dissolved；
4) in the environment of the mixed solution of step 3 being then placed in 35-40 DEG C, heating water bath, Raolical polymerizable are carried out
Completely, required hydrogel can be prepared；
5) surface is cleaned multiple times with distilled water in hydrogel made from step 4, removes the unreacted impurity in surface.
2. a kind of sodium lignin sulfonate aquagel according to claim 1 and preparation method thereof, it is characterised in that:
The vinyl polymerization monomer includes one or several kinds of in acrylic acid, acrylamide, vinyl alcohol and vinyl pyrrolidone mixes
Close object.
3. a kind of sodium lignin sulfonate aquagel according to claim 1 and preparation method thereof, it is characterised in that:
The crosslinking agent includes N, N '-methylene-bisacrylamide, ethylene glycol dimethacrylate, divinylbenzene and diisocyanate
One or several kinds of mixture in ester.
4. a kind of sodium lignin sulfonate aquagel according to claim 1 and preparation method thereof, it is characterised in that:
The initiator includes mixture one or several kinds of in hydrogen peroxide, ascorbic acid, potassium peroxydisulfate and ammonium persulfate.
5. a kind of sodium lignin sulfonate aquagel, it is characterised in that: it is by the described in any item preparations of claim 1-4
Method is made.
6. a kind of sodium lignin sulfonate aquagel according to claim 5, it is characterised in that: the hydrogel of preparation
Middle lignin sulfonic acid sodium content accounts for the 5-30% of overall solid content.
7. a kind of sodium lignin sulfonate aquagel according to claim 5, it is characterised in that: the hydrogel of preparation
Middle chitosan content accounts for the 8-10% of overall solid content.
8. a kind of sodium lignin sulfonate aquagel according to claim 5, it is characterised in that: the hydrogel of preparation
Middle content of crosslinking agent accounts for the 0.5-1% of overall solid content.
9. a kind of sodium lignin sulfonate aquagel according to claim 5, it is characterised in that: the hydrogel of preparation
The content of middle polymer accounts for the 65-95% of overall solid content.
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| CN114106367A (en) * | 2021-12-27 | 2022-03-01 | 浙江工业大学 | Biomass fully-degradable high-antibacterial high-water-absorptivity resin and preparation method thereof |
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Application publication date: 20190618 |