CN110204777A - A kind of preparation method of alginic acid composite hydrogel - Google Patents
A kind of preparation method of alginic acid composite hydrogel Download PDFInfo
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- CN110204777A CN110204777A CN201910592221.5A CN201910592221A CN110204777A CN 110204777 A CN110204777 A CN 110204777A CN 201910592221 A CN201910592221 A CN 201910592221A CN 110204777 A CN110204777 A CN 110204777A
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- sodium alginate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/10—Aqueous solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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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
- 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
- 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
Abstract
The preparation and preparation method thereof based on natural polysaccharide sodium alginate and synthesis macromolecule composite hydrogel that the present invention relates to a kind of.Using sodium alginate as raw material, using acrylic acid as monomer, ammonium persulfate is initiator, is added simultaneouslyN,N'-methylene-bisacrylamide is crosslinking agent.Alginic acid/polyacrylic acid inierpeneirating network structure composite hydrogel is prepared for by free radical solution polymerization.Products therefrom is transparent, and water absorption rate can reach 180g/g, and Water-saving effect is good.It is expected to be applied in fields such as biological medicine, new material, environmental protection and water conservations.
Description
Technical field
The invention belongs to advanced composite material (ACM) technical fields, are related to a kind of preparation of the polysaccharide composite hydrogel of high water absorbing capacity
Method.
Background technique
Hydrogel is a kind of high molecular material with three-dimensional net structure being cross-linked to form by hydrophilic high mol, can be in water
The middle a large amount of water of absorption does not dissolve but in water, soft and high resilience.Different technologies of preparing is taken, block can be obtained
Shape, membranaceous and nanoscale hydrogel.Water imbibition, water-retaining property and unique adsorptivity based on hydrogel, therefore we
It is dedicated to researching and developing a kind of aquagel with high water absorbing capacity based on boiomacromolecule.
Alginic acid is the naturally occurring colloid hy-drophilic polysaccharide extracted from seaweed, and abundance is degradable, is had good
Good biocompatibility and degradability.Contain the strong parent such as a large amount of reactive carboxyls, hydroxyl and carboxylate in alginic acid structure
Water base group.For polyacrylic acid as a kind of water-soluble macromolecule, main chain contains a large amount of carboxyl, therefore occurs in different pH environment
Reversible ionization-deionization process influences the hydrophily and swellability of hydrogel, realizes the responding ability to environment pH.
The present invention is using sodium alginate as raw material, using acrylic acid as monomer, and causes acroleic acid polymerization with ammonium persulfate, meanwhile, it is addedN, N'-methylene-bisacrylamide cross linked polyacrylate is prepared for alginic acid/polyacrylic acid composite hydrogel.Products therefrom is transparent,
Water absorption rate can reach 180g/g, and Water-saving effect is good.
The present invention is prepared for a kind of high water absorbing capacity composite high-molecular hydrogel based on alginic acid, and preparation method is simple, can
Strong operability.Meanwhile the water absorption rate and water retention of hydrogel are adjusted by different raw material proportioning, be retained it in environment,
The fields such as sewage treatment, separation and absorption have application value product more outstanding with natural polysaccharide and synthesis macromolecule for original
The hydrogel of material, formation has good biocompatibility and water suction, Water-saving effect, can be used as tissue engineering material, water conservation
Agent material etc..
Summary of the invention
The object of the present invention is to provide a kind of preparation sides that high water absorbing capacity composite hydrogel is prepared using sodium alginate as raw material
Method.
(1) preparation of alginic acid composite hydrogel
The present invention is preferable with biocompatibility, and the sodium alginate with good degradability is raw material, is single with acrylic acid
Body, is prepared for alginic acid composite hydrogel by way of free radical solution polymerization, and specific preparation method is as follows.
A. the preparation of sodium alginate soln.It disperses 1g sodium alginate (Al) in 100mL distilled water, 40 DEG C of stirrings are extremely
It is completely dissolved, is configured to sodium alginate soln.
B. gel-forming.Acrylic acid, initiator and crosslinking agent are added in the sodium alginate soln that step A is obtained, stirs
Mix 30min.Wherein, the quality proportioning of sodium alginate and acrylic acid (AA) are 1:4 ~ 1:20；Initiator is ammonium persulfate (APS),
Dosage is 0.025 ~ 0.100g；Crosslinking agent isN,N'-methylene-bisacrylamide (BIS), dosage are 0.025 ~ 0.100g；N, N'-methylene-bisacrylamide and initiator ammonium persulfate are previously dissolved in 1mL distilled water, and inject reactor with syringe.It is molten
Liquid is heated to 65 DEG C, stirs 1h, then 80 DEG C of 2 h of standing are to get composite hydrogel.
C. it is dehydrated and dry.Bulk hydrogel made from step B is soaked in 50mL distilled water, removes unreacted list
Body and other small molecules, replacement in each 24 hours distilled water 1 time.So operation 7 ~ 8 times.Then, it is soaked in the anhydrous second of 30mL
It is dehydrated in alcohol, every replacement in 4 hours dehydrated alcohol 1 time, repetitive operation 10 ~ 12 times.Hydrogel vacuum drying, forms hard block
Shape object.20 ~ 50 DEG C of vacuum drying temperature.
(2) morphology characterization of alginic acid composite hydrogel
It is observed by the means of scanning electron microscope to preparing alginic acid composite hydrogel pattern.Fig. 1 is alginic acid
The scanning electron microscope (SEM) photograph of composite hydrogel.The results show that the overall structure of hydrogel is stronger, there is the poroid knot of most network
Structure, and accumulated by bead, rough surface, large specific surface area, bore dia is between 100nm ~ 1 μm.These features are all said
Bright hydrone easily enters the inside of the hydrogel, therefore its water absorption rate is larger, in environment water conservation, sewage treatment, separation and suction
Attached equal fields have potential application.
Detailed description of the invention
Fig. 1 is a kind of alginic acid composite hydrogel scanning electron microscope (SEM) photograph involved in the present invention.
Specific embodiment
A kind of preparation method of alginic acid composite hydrogel of the present invention is carried out below by specific embodiment further
Explanation.
[embodiment 1]
1 g sodium alginate is dissolved in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe successively by 0.6mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 86.2g/g.
[embodiment 2]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 0.8mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 180.1g/g.
[embodiment 3]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 173.4g/g.
[embodiment 4]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.2mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 116.2g/g.
[embodiment 5]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.6mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 123.6g/g.
[embodiment 6]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 2.0mL AA, 1mL0.05g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 66.5g/g.
[embodiment 7]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.025g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 189.4g/g.
[embodiment 8]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.075g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 57.9g/g.
[embodiment 9]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.1g/mL BIS solution and
1mL0.05g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 36.8g/g.
[embodiment 10]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.05g/mL BIS solution and
1mL0.025g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 104.9g/g.
[embodiment 11]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.05g/mL BIS solution and
1mL0.075g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h,
80 DEG C are then heated to, 2 h are stood.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is answered
Heshui gel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard tiny is formed after vacuum dried
Grain, water absorption rate reach 118.4g/g.
[embodiment 12]
1 g sodium alginate is scattered in 100mL distilled water, and 40 DEG C of stirrings are to being completely dissolved.Take 10mL sodium alginate soln
In 50 mL there-necked flasks, nitrogen protection.With syringe be injected separately into 1.0mL AA, 1mL0.05g/mL BIS solution and
1mL0.1g/mL APS solution injects in 10mL sodium alginate soln.After stirring 30min, 65 DEG C are heated to, continues to stir 1h, so
After be warming up to 80 DEG C, stand 2 h.Up to alginic acid/polyacrylic acid composite hydrogel (Al/PAA).Alginic acid obtained is compound
Hydrogel is purified and is dehydrated to get pure transparent Al/PAA hydrogel.Hard fine particle is formed after vacuum dried,
Water absorption rate reaches 96.6g/g.
Claims (2)
1. a kind of preparation of alginic acid composite hydrogel, it is characterised in that:
The alginic acid composite hydrogel is by obtaining block by cross-linking reaction after sodium alginate, acrylic acid and crosslinking agent three mixing
Shape interpenetrating networks alginic acid/polyacrylic acid composite hydrogel；Products therefrom is transparent, by adjusting matching for acrylic acid and sodium alginate
Than the composite hydrogel of available different water absorption rates, water absorption rate is up to 180g/g；It is synthesized by following steps:
A. the preparation of sodium alginate aqueous solution: sodium alginate is dissolved in distilled water, and 40 DEG C of stirrings are to being completely dissolved；
B. acrylic acid, initiator and crosslinking agent, stirring gel-forming: are added in the sodium alginate soln that step A is obtained
30min；C. step B acquired solution is heated to 65 DEG C, heating stirring 1h, 80 DEG C of 2 h of standing obtain blocky gel；
C. be dehydrated and dry: bulk hydrogel made from step B is soaked in distilled water, remove unreacted monomer and its
His small molecule；Then it is soaked in dehydrated alcohol and is dehydrated, pure transparent hydrogel can be obtained；Pure transparent hydrogel is true
Sky is dry, forms hard block.
2. according to preparation method described in right 1, it is characterized in that:
100mL distilled water is added in 1g sodium alginate (Al) in step A, and 1h ~ 2h is stirred under the conditions of 40 DEG C of temperature；
The quality proportioning of sodium alginate and acrylic acid (AA) are 1:4 ~ 1:20 in step B；
Crosslinking agent in step BN,N'-methylene-bisacrylamide (BIS) dosage is 0.025 ~ 0.100g；Initiator ammonium persulfate
(APS) dosage is 0.025 ~ 0.100g.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111167423A (en) * | 2020-01-29 | 2020-05-19 | 兰州理工大学 | Preparation method and application of sodium alginate-sodium polyacrylate/sepiolite hydrogel |
| CN111370782A (en) * | 2020-03-20 | 2020-07-03 | 湖南源达新材料有限公司 | Long-life zinc-nickel battery and preparation method thereof |
| CN112274571A (en) * | 2020-12-02 | 2021-01-29 | 西安医学院 | Antibacterial hydrogel suitable for diabetic foot ulcer and preparation method thereof |
| CN113388405A (en) * | 2021-06-15 | 2021-09-14 | 鲁东大学 | Application of double-network hydrogel in soil water retention |
| CN114479122A (en) * | 2022-01-20 | 2022-05-13 | 西南石油大学 | Biomass hydrogel, preparation method and application |
| CN115251071A (en) * | 2022-08-12 | 2022-11-01 | 中国热带农业科学院橡胶研究所 | Sandwich type antibacterial water-retaining agent and preparation method thereof |
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| CN114479122A (en) * | 2022-01-20 | 2022-05-13 | 西南石油大学 | Biomass hydrogel, preparation method and application |
| CN115251071A (en) * | 2022-08-12 | 2022-11-01 | 中国热带农业科学院橡胶研究所 | Sandwich type antibacterial water-retaining agent and preparation method thereof |
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