CN106432611A - Chitosan quaternary ammonium salt grafting poly(acrylic-co-acrylamide) super-absorbent gel as well as preparation method and application thereof - Google Patents
Chitosan quaternary ammonium salt grafting poly(acrylic-co-acrylamide) super-absorbent gel as well as preparation method and application thereof Download PDFInfo
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- CN106432611A CN106432611A CN201610817405.3A CN201610817405A CN106432611A CN 106432611 A CN106432611 A CN 106432611A CN 201610817405 A CN201610817405 A CN 201610817405A CN 106432611 A CN106432611 A CN 106432611A
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Abstract
The invention belongs to the technical field of functional polymers, and particularly relates to chitosan quaternary ammonium salt grafting poly(acrylic-co-acrylamide) super-absorbent gel as well as a preparation method and an application thereof. The super-absorbent gel is a novel super-absorbent gel which is prepared by adopting chitosan quaternary ammonium salt, acrylic acid and acrylamide as raw materials, through a graft copolymerization and crosslinking reaction under the action of an initiator and a crosslinking agent, wherein content of the chitosan quaternary ammonium salt is 6.5%-75% of the total mass of the two monomers, namely the acrylic acid and the acrylamide, and content of the acrylamide is 10%-70% of the total mass of the two monomers, namely the acrylic acid and the acrylamide. The chitosan quaternary ammonium salt grafting poly(acrylic-co-acrylamide) super-absorbent gel has excellent water-absorbent, saline-absorbent, mechanical and anti-bacterial performances, and can be applicable to the technical field of personal hygiene materials.
Description
Technical field
The invention belongs to functional polymer technical field and in particular to a kind of chitosan quaternary ammonium salt grafting poly- (acrylic acid-
Co- acrylamide) superabsorbent hydrogel and its preparation method and application.
Background technology
Superabsorbent hydrogel is the crosslinked hydrophilic polymer of 3 D stereo, can absorb and will not dissolve while a large amount of water,
And partial gel has different responses to outside stimulus.As a kind of soft material, superabsorbent hydrogel has above-mentioned typically firm
The performance that property material does not possess, this makes it have special application advantage.Therefore, be widely used in living-hygienic articles for use, medical treatment,
The field such as agricultural gardening and sewage disposal.However, the partial properties of superabsorbent hydrogel are also to be strengthened, to expand further
Its range of application.
Traditional superabsorbent hydrogel is typically by synthesis macromolecule preparation, but its biological degradability is not enough.With current social pair
The pay attention to day by day of the feature of environmental protection, preparing superabsorbent hydrogel using the natural polymer with good biodegradability properties has become a weight
Want trend.Wherein, the superabsorbent hydrogel of the preparation such as cellulose and starch has preferable water absorbing properties and biological degradability, is one
The environmentally friendly raw material of class.But because the demand that people's opposite applies flexibly quality improves constantly, to superabsorbent hydrogel
Other performance it is also proposed new requirement, for example, have the performances such as certain antibacterial and mechanics.In order to increase superabsorbent hydrogel
Superabsorbent hydrogel is typically additionally mixed or adsorbs some small molecule antiseptics by bacteriostasis property, as silver-colored in inorganic metal or organic
Aldehydes etc..Shitosan as a kind of natural biodegradable polymer, then to bacterial growth after antibacterial group is introduced on its strand
There is certain inhibition, therefore, it can for chitosan derivatives preparation to become antibiotic property degradable superabsorbent hydrogel.Additionally,
Shitosan is only dissolved in weak acid so as to all receive certain restriction in the preparation and application of material.Chitosan quaternary ammonium salt is
A kind of chitosan derivatives introducing quaternary ammonium salt group, not only possess chitosan biological compatible and degradable the advantages of, and
Significantly improve the water solubility of shitosan, there is the performances such as good antibacterial and absorption, be expected to be applied to daily use chemicals, medicine and food
In field.
Content of the invention
The present invention be directed to the deficiencies in the prior art it is therefore intended that provide a kind of have excellent water suction, inhale salt solution, mechanics and
Chitosan quaternary ammonium salt grafting poly- (acrylic-co-acrylamide) superabsorbent hydrogel of anti-microbial property and its preparation method and application.
For achieving the above object, the technical solution used in the present invention is：
A kind of chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel, by chitosan quaternary ammonium salt,
Acrylic acid and acrylamide are prepared from the presence of initiator and crosslinking agent, and the consumption of described chitosan quaternary ammonium salt is propylene
Acid and the 6.5%～75% of two kinds of monomer gross mass of acrylamide.
In such scheme, the consumption of described acrylamide be acrylic acid and two kinds of monomer gross mass of acrylamide 10%～
70%.
In such scheme, described initiator is potassium peroxydisulfate.
In such scheme, the consumption of described initiator be acrylic acid and two kinds of monomer gross mass of acrylamide 0.25%～
1.25%.
In such scheme, described crosslinking agent is N, N'- methylene-bisacrylamide.
In such scheme, the consumption of described crosslinking agent be acrylic acid and two kinds of monomer gross mass of acrylamide 0.05%～
0.30%.
Above-mentioned chitosan quaternary ammonium salt is grafted the preparation method of poly- (acrylic-co-acrylamide) superabsorbent hydrogel, including such as
Lower step：
(1) chitosan quaternary ammonium salt is added to the water, is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
(2) under condition of ice bath, with NaOH, acrylic acid is carried out with titration neutralization；
(3) after neutralization terminates, then add acrylamide toward in acrylic acid solution, be sufficiently mixed uniformly；
(4) mixed solution of step (3) gained acrylic acid and acrylamide is added to chitosan quaternary ammonium salting liquid, mix
Close uniformly；It is added thereto to initiator solution again, under nitrogen protection, carry out pre- initiation in uniform temperature；It is subsequently adding crosslinking agent molten
Liquid, is heated to uniform temperature under nitrogen protection and carries out cross-linking reaction；
(5) reaction terminate after, by gained gel detergent, be dried after obtain chitosan quaternary ammonium salt grafting poly- (acrylic acid-
Co- acrylamide) superabsorbent hydrogel.
In such scheme, the temperature of the described pre- initiation of step (4) is 30 DEG C, and the time is 15 minutes.
In such scheme, the temperature of the described cross-linking reaction of step (4) is 65 DEG C, and the reaction time is 3 hours.
In such scheme, the described drying of step (5) is freeze-drying or drying, and the temperature of described drying is less than 60 DEG C.
Above-mentioned chitosan quaternary ammonium salt grafting poly- (acrylic-co-acrylamide) superabsorbent hydrogel is led in personal hygiene material
The application in domain.
Beneficial effects of the present invention：(1) present invention, with chitosan quaternary ammonium salt, acrylic acid and acrylamide as raw material, passes through
Graft copolymerization and cross-linking reaction obtain a kind of new superabsorbent hydrogel, described superabsorbent hydrogel have excellent water suction, inhale salt solution,
Mechanics and anti-microbial property；(2) chitosan quaternary ammonium salt of the present invention is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Water suction, inhale salt solution, mechanics and anti-microbial property can use needs according to difference, by adjust chitosan quaternary ammonium salt, acrylic acid and
The consumption of acrylamide, initiator and dosage of crosslinking agent are regulated and controled, and can meet different specifically used demands；(3) this
Bright described chitosan quaternary ammonium salt grafting poly- (acrylic-co-acrylamide) superabsorbent hydrogel is due to introducing natural polymer, material
Material has degradability, thus decreasing environmental pollution；(4) chitosan quaternary ammonium salt of the present invention is grafted poly- (acrylic acid-co-
Acrylamide) superabsorbent hydrogel can be used for personal hygiene Material Field；(5) preparation process is simple of the present invention, low cost, are expected to reality
Existing commercial application.
Brief description
Fig. 1 is the synthesis that in the present invention, chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Journey and microstructure schematic diagram.
Fig. 2 is the scanning electricity that in the present invention, chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Mirror figure.
Specific embodiment
For a better understanding of the present invention, it is further elucidated with present disclosure with reference to embodiment, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
A kind of chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel, is prepared via a method which
Obtain：
(1) chitosan quaternary ammonium salt (consumption is the 12.5% of acrylic acid and two kinds of monomer gross mass of acrylamide) is added to
In water, it is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
(2) with NaOH, acrylic acid is carried out in ice bath with titration neutralization；
(3) (acrylamide consumption is two kinds of monomer gross mass to add acrylamide toward in above-mentioned gained acrylic acid solution
10%), it is sufficiently mixed uniformly；
(4) acrylic acid and acrylamide mixed solution are added to chitosan quaternary ammonium salting liquid, mix；Added
Potassium sulfate (consumption is the 1.0% of acrylic acid and two kinds of monomer gross mass of acrylamide) solution, draws in advance in 30 DEG C under nitrogen protection
Send out 15 minutes；It is subsequently adding N, (consumption is acrylic acid and two kinds of monomer gross mass of acrylamide to N'- methylene-bisacrylamide
0.2%) solution, reacts 3 hours in 65 DEG C under nitrogen protection；
(5) after reaction terminates, by the gel detergent obtaining, can get chitosan quaternary ammonium salt grafting after freeze-drying poly-
(acrylic-co-acrylamide) superabsorbent hydrogel.
The water absorbing properties of superabsorbent hydrogel are tested using weight method, and water absorption rate is pressed formula (1) and calculated：
WeFor superabsorbent hydrogel weight (g) during water suction balance, W0For the dry state superabsorbent hydrogel initial mass before water suction
G (), absorption salt ratio is also pressed formula (1) and is calculated.
The present embodiment prepares the suction that chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Water rate reaches 774g/g, and absorption salt ratio is 88g/g, and it is excellent that result shows that the introducing of acrylamide causes this superabsorbent hydrogel to have
Water suction and inhale salt solution performance.
Fig. 1 is grafted poly- (acrylic-co-acrylamide) superabsorbent water-setting for the chitosan quaternary ammonium salt that the present embodiment prepares
The building-up process of glue and microstructure schematic diagram, chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Scanning electron microscope (SEM) photograph see Fig. 2.As can be seen from Figure 1：Using the acrylamide monomer containing non-ionic groups with contain ion
Copolymerization between the acrylic monomers of type group, has been grafted poly- (acrylic-co-acrylamide) copolymerization on chitosan quaternary ammonium salt
Thing, by the crosslinked action of poly- (acrylic-co-acrylamide) copolymer molecule interchain, generates a kind of new superabsorbent water-setting
Glue.The scanning electron microscope (SEM) photograph that the chitosan quaternary ammonium salt of Fig. 2 is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel shows, due to
The introducing of acrylamide, this superabsorbent hydrogel has uniformly three-dimensional porous dimensional network structure.
Embodiment 2
A kind of chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel, is prepared via a method which
Obtain：
(1) chitosan quaternary ammonium salt (consumption is the 12.5% of acrylic acid and two kinds of monomer gross mass of acrylamide) is added to
In water, it is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
(2) with NaOH, acrylic acid is carried out in ice bath with titration neutralization；
(3) (acrylamide and acrylic acid consumption respectively account for total list to add acrylamide toward in above-mentioned gained acrylic acid solution
The 50% of weight), it is sufficiently mixed uniformly；
(4) acrylic acid and acrylamide mixed solution are added to chitosan quaternary ammonium salting liquid, mix；Added
Potassium sulfate (consumption is the 1.0% of acrylic acid and two kinds of monomer gross mass of acrylamide) solution, draws in advance in 30 DEG C under nitrogen protection
Send out 15 minutes；It is subsequently adding N, (consumption is acrylic acid and two kinds of monomer gross mass of acrylamide to N'- methylene-bisacrylamide
0.2%) solution, reacts 3 hours in 65 DEG C under nitrogen protection；
(5) after reaction terminates, by the gel detergent obtaining, can get chitosan quaternary ammonium salt grafting after freeze-drying poly-
(acrylic-co-acrylamide) superabsorbent hydrogel.
The present embodiment prepares chitosan quaternary ammonium salt and is grafted the anti-of poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Pressure performance reaches 26KPa, and result shows that the introducing of acrylamide causes this superabsorbent hydrogel to have good mechanical property.
Embodiment 3
A kind of chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel, is prepared via a method which
Obtain：
(1) chitosan quaternary ammonium salt (consumption is the 62.5% of acrylic acid and two kinds of monomer gross mass of acrylamide) is added to
In water, it is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
(2) with NaOH, acrylic acid is carried out in ice bath with titration neutralization；
(3) (acrylamide and acrylic acid consumption respectively account for total list to add acrylamide toward in above-mentioned gained acrylic acid solution
The 50% of weight), it is sufficiently mixed uniformly；
(4) acrylic acid and acrylamide mixed solution are added to chitosan quaternary ammonium salting liquid, mix；Added
Potassium sulfate (consumption is the 0.75% of acrylic acid and two kinds of monomer gross mass of acrylamide) solution, draws in advance in 30 DEG C under nitrogen protection
Send out 15 minutes；It is subsequently adding N, (consumption is acrylic acid and two kinds of monomer gross mass of acrylamide to N'- methylene-bisacrylamide
0.2%) solution, reacts 3 hours in 65 DEG C under nitrogen protection；
(5) after reaction terminates, by the gel detergent obtaining, can get chitosan quaternary ammonium salt grafting after freeze-drying poly-
(acrylic-co-acrylamide) superabsorbent hydrogel.
The anti-microbial property of superabsorbent hydrogel is tested using absorbance method, and bacteriostasis rate is pressed formula (2) and calculated：
A0Not plus superabsorbent hydrogel bacteria culture media absorbance, A be add superabsorbent hydrogel bacteria culture media extinction
Degree.
The present embodiment prepares chitosan quaternary ammonium salt and is grafted the anti-of poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Bacterium results of property shows, reaches 40% to colibacillary bacteriostasis rate.
Embodiment 4
A kind of chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel, is prepared via a method which
Obtain：
(1) chitosan quaternary ammonium salt (consumption is the 25% of acrylic acid and two kinds of monomer gross mass of acrylamide) is added to water
In, it is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
(2) with NaOH, acrylic acid is carried out in ice bath with titration neutralization；
(3) (consumption of acrylic acid and acrylamide respectively accounts for total list to add acrylamide toward in above-mentioned gained acrylic acid solution
The 50% of weight), it is sufficiently mixed uniformly；
(4) acrylic acid and acrylamide mixed solution are added to chitosan quaternary ammonium salting liquid, mix；Added
Potassium sulfate (consumption is the 0.75% of acrylic acid and two kinds of monomer gross mass of acrylamide) solution, draws in advance in 30 DEG C under nitrogen protection
Send out 15 minutes；It is subsequently adding N, (consumption is acrylic acid and two kinds of monomer gross mass of acrylamide to N'- methylene-bisacrylamide
0.1%) solution, reacts 3 hours in 65 DEG C under nitrogen protection；
(5) after reaction terminates, by the gel detergent obtaining, after drying, can get chitosan quaternary ammonium salt grafting less than 60 DEG C
Poly- (acrylic-co-acrylamide) superabsorbent hydrogel.
The present embodiment prepares the suction that chitosan quaternary ammonium salt is grafted poly- (acrylic-co-acrylamide) superabsorbent hydrogel
Water rate is 544g/g；Anti-microbial property result shows, reaches 37.8% to colibacillary bacteriostasis rate.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and the not restriction to embodiment.Right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change therefore amplified or change
Move within still in the protection domain of the invention.
Claims (10)
1. a kind of chitosan quaternary ammonium salt grafting is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel is it is characterised in that gathered by shell
Sugared quaternary ammonium salt, acrylic acid and acrylamide are prepared from the presence of initiator and crosslinking agent, described chitosan quaternary ammonium salt
Consumption is the 6.5% ~ 75% of acrylic acid and two kinds of monomer gross mass of acrylamide.
2. chitosan quaternary ammonium salt grafting according to claim 1 is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel, its
It is characterised by, the consumption of described acrylamide is the 10% ~ 70% of acrylic acid and two kinds of monomer gross mass of acrylamide.
3. chitosan quaternary ammonium salt grafting according to claim 1 is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel, its
It is characterised by, described initiator is potassium peroxydisulfate.
4. chitosan quaternary ammonium salt grafting according to claim 1 is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel, its
It is characterised by, the consumption of described initiator is the 0.25% ~ 1.25% of acrylic acid and two kinds of monomer gross mass of acrylamide.
5. chitosan quaternary ammonium salt grafting according to claim 1 is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel, its
It is characterised by, described crosslinking agent is N, N'- methylene-bisacrylamide.
6. chitosan quaternary ammonium salt grafting according to claim 1 is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel, its
It is characterised by, the consumption of described crosslinking agent is the 0.05% ~ 0.30% of acrylic acid and two kinds of monomer gross mass of acrylamide.
7. the arbitrary described chitosan quaternary ammonium salt grafting of claim 1 ~ 6 is poly-（Acrylic acid-co- acrylamide）The system of superabsorbent hydrogel
Preparation Method is it is characterised in that comprise the steps：
（1）Chitosan quaternary ammonium salt is added to the water, is sufficiently stirred for making it after dissolving, obtain chitosan quaternary ammonium salting liquid；
（2）Under condition of ice bath, with NaOH, acrylic acid is carried out with titration neutralization；
（3）After neutralization terminates, then add acrylamide toward in acrylic acid solution, be sufficiently mixed uniformly；
（4）By step（3）The mixed solution of gained acrylic acid and acrylamide adds to chitosan quaternary ammonium salting liquid, and mixing is all
Even；It is added thereto to initiator solution again, under nitrogen protection, carry out pre- initiation in uniform temperature；It is subsequently adding cross-linking agent solution,
It is heated to uniform temperature under nitrogen protection and carry out cross-linking reaction；
（5）After reaction terminates, poly- by obtaining chitosan quaternary ammonium salt grafting after gained gel detergent, drying（Acrylic acid-co- the third
Acrylamide）Superabsorbent hydrogel.
8. according to claim 7 preparation method it is characterised in that step（4）The temperature of described pre- initiation is 30 DEG C, the time
For 15 minutes.
9. according to claim 7 preparation method it is characterised in that step（4）The temperature of described cross-linking reaction is 65 DEG C, instead
It is 3 hours between seasonable.
10. described in any one of claim 1 ~ 6, chitosan quaternary ammonium salt grafting is poly-（Acrylic acid-co- acrylamide）Superabsorbent hydrogel
Application in personal hygiene Material Field.
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Cited By (5)
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| CN107955099A (en) * | 2017-12-26 | 2018-04-24 | 安徽省东乾食品有限公司 | A kind of preparation method of the absorbing membrane based on vegetable and fruit packaging |
| CN112961281A (en) * | 2020-08-11 | 2021-06-15 | 李方 | High-salt-tolerance super absorbent resin |
| CN114042383A (en) * | 2021-12-16 | 2022-02-15 | 中国海洋大学 | Super-hydrophilic chitosan quaternary ammonium salt hydrogel composite membrane and preparation method and application thereof |
| CN114276493A (en) * | 2022-03-03 | 2022-04-05 | 河南博源新材料有限公司 | Preparation method of composite polyacrylamide |
| CN117304547A (en) * | 2023-09-14 | 2023-12-29 | 海南医学院第一附属医院 | Polyacrylamide-quaternized chitosan/EGCG hydrogel, preparation method thereof and application thereof in back wound healing |
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| CN104987461A (en) * | 2015-07-31 | 2015-10-21 | 浙江金壳药业有限公司 | Chitosan derivative antibacterial superabsorbent gel and preparation method therefor |
| CN105254811A (en) * | 2015-11-10 | 2016-01-20 | 陕西科技大学 | Carboxymethyl chitosan quaternary ammonium salt and preparation method thereof |
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| CN104356303A (en) * | 2014-11-24 | 2015-02-18 | 张家港保税区冠祥贸易有限公司 | Preparation method for natural high-antibacterial-property water-absorbent resin |
| CN104987461A (en) * | 2015-07-31 | 2015-10-21 | 浙江金壳药业有限公司 | Chitosan derivative antibacterial superabsorbent gel and preparation method therefor |
| CN105254811A (en) * | 2015-11-10 | 2016-01-20 | 陕西科技大学 | Carboxymethyl chitosan quaternary ammonium salt and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107955099A (en) * | 2017-12-26 | 2018-04-24 | 安徽省东乾食品有限公司 | A kind of preparation method of the absorbing membrane based on vegetable and fruit packaging |
| CN112961281A (en) * | 2020-08-11 | 2021-06-15 | 李方 | High-salt-tolerance super absorbent resin |
| CN114042383A (en) * | 2021-12-16 | 2022-02-15 | 中国海洋大学 | Super-hydrophilic chitosan quaternary ammonium salt hydrogel composite membrane and preparation method and application thereof |
| CN114276493A (en) * | 2022-03-03 | 2022-04-05 | 河南博源新材料有限公司 | Preparation method of composite polyacrylamide |
| CN117304547A (en) * | 2023-09-14 | 2023-12-29 | 海南医学院第一附属医院 | Polyacrylamide-quaternized chitosan/EGCG hydrogel, preparation method thereof and application thereof in back wound healing |
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