CN105504166B - A kind of sodium alginate-acrylamide composite hydrogel and its preparation method and application - Google Patents
A kind of sodium alginate-acrylamide composite hydrogel and its preparation method and application Download PDFInfo
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- CN105504166B CN105504166B CN201610037390.9A CN201610037390A CN105504166B CN 105504166 B CN105504166 B CN 105504166B CN 201610037390 A CN201610037390 A CN 201610037390A CN 105504166 B CN105504166 B CN 105504166B
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- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The invention discloses a kind of sodium alginate acrylamide composite hydrogel, preparation method includes the following steps：1) it is sodium alginate and acrylamide is soluble in water uniformly mixed in proportion；2) crosslinking agent is sequentially added, initiator is added in after carrying out froth in vacuum processing, addition catalyst；3) gained mixed liquor is transferred to heating in glass mold to react to get the sodium alginate acrylamide composite hydrogel.Sodium alginate acrylamide composite hydrogel of the present invention has preferable multivalent ion adsorption capacity and biocompatibility；It is acted on reference to the graft copolymerization of polyacrylamide network and sodium alginate and acrylamide, the mechanical property of gained hydrogel is made effectively to be promoted；And the hydrogel has sensibility under different pH, can generate intermolecular interaction, the fields such as adsorbing separation and sewage disposal suitable for chemical substance with a variety of dyes of positive ion and heavy metal ion.
Description
Technical field
The invention belongs to environment-friendly materials fields, and in particular to a kind of sodium alginate-acrylamide composite hydrogel and its system
Preparation Method and application.
Background technology
With industrial development, urbanization speed-raising and the expansion of the size of population, China is faced with the water environment of very severe
Situation.In recent years, Chinese great environmental pollution and accident occurred again and again, and wherein water pollution accident accounts for half or so.According to supervision
Portion's statistical analysis, for the annual water pollution accident in China all at 1700 or more, water pollution has seriously affected the production of the people
Life.On April 16th, 2015, State Council formally issues《Water prevention and cure of pollution action plan》, " ten, water " is put into effect.About water pollution
The reason of serious, is mainly influenced by three factors, first, industrial pollution；Second is that city domestic sewage；Third, pollution of area source, i.e. agriculture
Apply chemical fertilizer, pesticide and the pollutions such as nitrogen, phosphorus caused by soil erosion in field.The discharge of industrial wastewater is cause water pollution main
Reason.It is primarily due to contain in industrial wastewater there are many harmful heavy metal ion (such as chromium, cadmium, copper, mercury, nickel, zinc), these
If ion processing, which is not thorough, can bring serious ecological problem, such as " minamata disease " and " itai-itai ".Therefore, a huge sum of money in sewage
The removing for belonging to ion is the important subject of sewage disposal.
Absorption method has effluent containing heavy metal ions good removal efficiency, can effectively recycle micro heavy in waste water
Etc. special advantages, be it is a kind of handle heavy metal ion important method.It is early had been reported that for heavy metal ion adsorbed hydrogel：
Wu Peng etc. is prepared for a kind of sodium alginate/cellulose aquagel ball, and the plural gel ball is to methylene blue, auramine O and Zang Hong T etc.
The dye of positive ion has good adsorption effect, and is to the adsorbance of methylene blue containing 50% sodium alginate gel ball
163.36mg/g (the preparation and application functional materials of Wu Peng, Liu Zhiming sodium alginate/cellulose aquagel ball, 2015,46
(10)：10144-10147)；Yuan Yihua etc. is prepared for a kind of cross-linked chitosan/sodium alginate adsorbent, to the Cu in water phase2+
With good adsorptivity (the research of the such as Yuan Yihua, Lei Li epoxychloropropane cross-linked chitosan/sodium alginate absorption copper ion
South China Science ＆ Engineering University's journal (natural science edition), 2012,40 (7):148-154).
Sodium alginate can be complexed well with divalent and more than metal ion, have preferable absorption property；It is but simple
Sodium alginate be easily swollen in water, poor mechanical property, which greatly limits the applications of sodium alginate.
Invention content
The object of the present invention is to provide a kind of sodium alginate-acrylamide composite hydrogel and its preparation method and application,
The sodium alginate-acrylamide composite hydrogel has preferable mechanical property and higher adsorption efficiency, can effectively adsorb weight
The harmful chemicals such as metal ion, the dye of positive ion for sewage disposal, also act as the fields such as tissue engineering bracket.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation method of sodium alginate-acrylamide composite hydrogel, it is as follows to specifically include step：
1) sodium alginate and acrylamide are pressed 1:The mass ratio of (5~12) is soluble in water, obtains uniform mixed liquor I；
2) crosslinking agent, initiator are added in mixed liquor I successively, addition catalyst must mix after carrying out froth in vacuum processing
Liquid II, wherein crosslinking agent, initiator, catalyst and acrylamide mass ratio be (0.05~5):(0.1~2):(0.2~
2.5):100；
3) gained mixed liquor I I is transferred in the glass mold of protective gas atmosphere, the insulation reaction 1 at 40~70 DEG C
~6h is to get the sodium alginate-acrylamide composite hydrogel；Gel taking-up is cut into homogeneous bulky, uses absolute ethyl alcohol
Replaced washing every 12 hours with deionized water, to remove the small molecules such as unreacted acrylamide, be freeze-dried to constant weight.
In said program, the total concentration of sodium alginate and acrylamide is 10~20wt% in the mixed liquor I.
In said program, the optional N of crosslinking agent, N '-methylene-bisacrylamide, N, N'- diallyls tartaric acid two
Amide, divinylbenzene, multicondensed ethylene glycol diacrylate or Polyethylene glycol dimethacrylate etc..
In said program, the optional ammonium persulfate of the initiator, potassium peroxydisulfate or sodium peroxydisulfate etc..
In said program, the optional sodium sulfite of the catalyst, sodium hydrogensulfite or sodium thiosulfate etc..
In said program, the vacuum defoamation treatment conditions are：Pressure is evacuated to as 0.02~0.005MPa, the time is
1~3h.
Preferably, insulation reaction time described in step 3) is 1.5~2.5h.
In said program, the protective gas is nitrogen or argon gas etc..
According to sodium alginate-acrylamide composite hydrogel prepared by said program, wherein acrylamide gathers with crosslinking agent
The hydrogel three-dimensional network being cross-linked to form is closed, sodium alginate linear molecule interts wherein；And sodium alginate occurs with acrylamide
Graft copolymerization, the amino on carboxyl and polyacrylamide on long-chain are crosslinked by forming amide group.Gained seaweed
The structure diagram of sour sodium-acrylamide composite hydrogel as shown in Figure 1, its interior joint 1. as shown in figure Chinese style (1), node is 2.
Shown in such as figure Chinese style (2).
Sodium alginate-acrylamide the composite hydrogel prepared according to said program can be used as the absorption of heavy metal ion
Agent, for adsorbing separation copper ion, mercury ion, cadmium ion, lead ion, zinc ion, barium ions, chromium ion, manganese ion, cobalt from
Son, nickel ion or tungsten ion etc..
Graft copolymerization of the sodium alginate of the present invention-acrylamide composite hydrogel for sodium alginate and acrylamide
Object, the hydrogel three-dimensional network that acrylamide is formed with crosslinking agent polymerization crosslinking；Sodium alginate linear molecule interts wherein, true
Under the conditions of empty anaerobic or few oxygen, the amino on carboxyl and polyacrylamide on long-chain is handed over by forming amide group
Connection；The froth in vacuum processing step can effectively remove the bubble in mixed solution, reduce the stress even avoided in hydrogel
Defect promotes its mechanical property；Oxygen in vacuum defoamation energy elimination reaction solution simultaneously, and initiation system is combined, promote sea
The cross-linking process of mosanom and acrylamide improves the mechanical property of gained hydrogel.
Beneficial effects of the present invention are：
1) single step reaction of the present invention, that is, plastic, the preparation process being related to is simple, can prepare variously-shaped hydrogel, and
Raw material sources are wide, of low cost.
2) de-bubble processing step of the present invention can effectively remove the bubble in mixed solution, make molding hydrogel will not
Stress defect is generated, effectively promotes its mechanical property；Vacuum defoamation simultaneously can remove the oxygen in solution, can effectively facilitate seaweed
The cross-linking process of sour sodium and acrylamide, and shorten the reaction time.
3) sodium alginate of the present invention-acrylamide composite hydrogel has good multivalent ion adsorption capacity and life
The features such as object compatibility；Sodium alginate is interspersed in polyacrylamide hydrogel three-dimensional network, and can realize sodium alginate simultaneously
With the graft copolymerization of acrylamide, make gained hydrogel that there is excellent mechanical property and swelling resistance.
4) present invention gained hydrogel has sensibility under different pH, can be with a variety of dyes of positive ion and heavy metal ion
Generate intermolecular interaction, the fields such as adsorbing separation and sewage disposal suitable for chemical substance.
Description of the drawings
Fig. 1 is the structure diagram of sodium alginate-acrylamide composite hydrogel.
Fig. 2 is 5 gained sodium alginate of the embodiment of the present invention-swelling of the acrylamide composite hydrogel under condition of different pH
Rate.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
Unless specific instructions, the reagent of use is commercially available chemical reagent or industrial products to following embodiment.
In following embodiment, the test method of swelling behavior is as follows：Sodium alginate-acrylamide obtained by the present invention is compound
The cylinder test specimen of diameter 1.0cm, high 1mm is made in hydrogel, is soaked in the buffering that pH is 2,4,6,8 after drying to constant weight respectively
In liquid (25 DEG C), its quality of periodic measurement, until reaching swelling equilibrium, to test its swelling behavior.
The test method of absorption property is as follows：Accurately weigh sodium alginate-propylene that 300mg is freeze-dried to constant weight
Amide composite hydrogel is added at 25 DEG C in the heavy metallic salt aqueous solution of a concentration of 5g/L of 100ml, carries out constant temperature oscillation, is used
Atomic absorption spectrum measures the adsorbance of heavy metal ion, up to adsorption equilibrium, calculates the maximal absorptive capacity of sample.
The test method of compression verification is as follows：Using universal testing machine (RGM-30A) to dry to constant weight, diameter,
The column sodium alginate-acrylamide composite hydrogel sample for being highly 10mm carries out compression verification, compressive deformation 50%,
Compression speed is 2mm/min.
Embodiment 1
A kind of sodium alginate-acrylamide composite hydrogel, preparation method include the following steps：
At room temperature by sodium alginate (SA) powder and acrylamide (AM) by 1:5 mass ratio is dissolved in ionized water, is obtained
Uniform mixed liquor I, the total concentration of sodium alginate and acrylamide is 11wt% in mixed liquor I；Sequentially add N, N'- diene
Propyl tartaric acid diamides and sodium peroxydisulfate carry out froth in vacuum processing and (are evacuated to 0.02MPa, the time is after dissolving
2h), it then adds in sodium hydrogensulfite to be uniformly mixed, wherein N, N'- diallyl tartardiamides, sodium peroxydisulfate, sulfurous acid
The mass ratio of hydrogen sodium and acrylamide monomer is respectively 3.85:0.9:1.55:100, acquired solution is then transferred to nitrogen gas
In the glass mold of atmosphere, it is compound that the sodium alginate-acrylamide is made in insulation reaction 2.5h, i.e. molding at 70 DEG C after sealing
Hydrogel.
The taking-up of molding sodium alginate-acrylamide composite hydrogel is cut into homogeneous bulky, with absolute ethyl alcohol and go from
Sub- water was alternately washed every 12 hours, was washed four days, and to remove the small molecules such as unreacted acrylamide, freeze-drying is dry extremely
Constant weight.
The present embodiment is subjected to absorption property to sodium alginate-acrylamide composite hydrogel obtained by constant weight through dry, is led to
It is 13.40mg/g to the adsorbance of copper ion to cross atomic absorption spectrum and measure in copper-bath (heavy metallic salt aqueous solution)；
When measuring (compression verification) shape by universal testing machine and becoming 50%, compressive strength 6.03MPa.
Embodiment 2
A kind of sodium alginate-acrylamide composite hydrogel, preparation method include the following steps：
At room temperature by sodium alginate (SA) powder and acrylamide (AM) by 1:7 mass ratio is dissolved in ionized water, is obtained
Uniform mixed liquor I, the total concentration of sodium alginate and acrylamide is 13wt% in mixed liquor I；Sequentially add divinyl
Benzene and potassium peroxydisulfate, froth in vacuum processing (being evacuated to 0.015MPa, time 1.3h) is carried out after dissolving, is then added in sub-
Sodium sulphate is uniformly mixed, and the mass ratio of wherein divinylbenzene, potassium peroxydisulfate, sodium sulfite and acrylamide monomer is respectively
2.95:1.9:2.35:100, then acquired solution is transferred in the glass mold of nitrogen atmosphere, is kept the temperature at 60 DEG C after sealing
6h is reacted, that is, is molded and the sodium alginate-acrylamide composite hydrogel is made.
The taking-up of molding sodium alginate-acrylamide composite hydrogel is cut into homogeneous bulky, with absolute ethyl alcohol and go from
Sub- water was alternately washed every 12 hours, is washed four days, to remove the small molecules such as unreacted acrylamide, is freeze-dried to perseverance
Weight.
The present embodiment is subjected to absorption property to sodium alginate-acrylamide composite hydrogel obtained by constant weight through dry, is led to
It is 17.13mg/g to the adsorbance of barium ions to cross atomic absorption spectrum and measure in barium chloride solution；Pass through universal material testing
When machine measures (compression verification) shape and becomes 50%, compressive strength 10.03MPa.
Embodiment 3
A kind of sodium alginate-acrylamide composite hydrogel, preparation method include the following steps：
At room temperature by sodium alginate (SA) powder and acrylamide (AM) by 1:9 mass ratio is dissolved in ionized water, is obtained
Uniform mixed liquor I, the total concentration of sodium alginate and acrylamide is 15wt% in mixed liquor I；Sequentially add more contracting second two
Alcohol diacrylate and sodium peroxydisulfate carry out froth in vacuum processing (being evacuated to 0.01MPa, time 2.5h) after dissolving,
Then it adds in sodium thiosulfate to be uniformly mixed, wherein multicondensed ethylene glycol diacrylate, sodium peroxydisulfate, sodium thiosulfate and propylene
The mass ratio of amide monomer is respectively 4.8:0.1:0.25:100, then acquired solution is transferred to the glass mold of argon gas atmosphere
In, the sodium alginate-acrylamide composite hydrogel is made in insulation reaction 4h, i.e. molding at 45 DEG C after sealing.
The taking-up of molding sodium alginate-acrylamide composite hydrogel is cut into homogeneous bulky, with absolute ethyl alcohol and go from
Sub- water was alternately washed every 12 hours, is washed four days, to remove the small molecules such as unreacted acrylamide, is freeze-dried to perseverance
Weight.
The present embodiment is subjected to absorption property to sodium alginate-acrylamide composite hydrogel obtained by constant weight through dry, is led to
Cross atomic absorption spectrum measure the zinc ion in liquor zinci chloridi adsorbance be 14.23mg/g；Pass through universal testing machine
When measuring (compression verification) shape and becoming 50%, compressive strength 15.52MPa.
Embodiment 4
A kind of sodium alginate-acrylamide composite hydrogel, preparation method include the following steps：
At room temperature by sodium alginate (SA) powder and acrylamide (AM) by 1:9 mass ratio is dissolved in ionized water, is obtained
Uniform mixed liquor I, the total concentration of sodium alginate and acrylamide is 15wt% in mixed liquor I；Sequentially add more contracting second two
Alcohol dimethylacrylate and potassium peroxydisulfate carry out froth in vacuum processing and (are evacuated to 0.0075MPa, the time is after dissolving
2.5h), it then adds in sodium hydrogensulfite to be uniformly mixed, wherein Polyethylene glycol dimethacrylate, potassium peroxydisulfate, sulfurous acid
The mass ratio of hydrogen sodium is respectively 2.1:0.25:0.5:100, then acquired solution is transferred in the glass mold of argon gas atmosphere,
The sodium alginate-acrylamide composite hydrogel is made in insulation reaction 3h, i.e. molding at 55 DEG C after sealing.
The taking-up of molding sodium alginate-acrylamide composite hydrogel is cut into homogeneous bulky, with absolute ethyl alcohol and go from
Sub- water was alternately washed every 12 hours, is washed four days, to remove the small molecules such as unreacted acrylamide, is freeze-dried to perseverance
Weight.
The present embodiment is subjected to absorption property to sodium alginate-acrylamide composite hydrogel obtained by constant weight through dry, is led to
Cross atomic absorption spectrum measured in nitric acid cadmium solution cadmium ion adsorbance be 17.34mg/g；Pass through universal testing machine
When measuring (compression verification) shape and becoming 50%, compressive strength 12.33MPa.
Embodiment 5
A kind of sodium alginate-acrylamide composite hydrogel, preparation method include the following steps：
At room temperature by sodium alginate (SA) powder and acrylamide (AM) by 1:8 mass ratio is dissolved in ionized water, is obtained
Uniform mixed liquor I, the total concentration of sodium alginate and acrylamide is 17wt% in mixed liquor I；Sequentially add N, N '-methylene
Base bisacrylamide (BIS) and ammonium persulfate ((NH4)2S2O8), it carries out froth in vacuum processing after dissolving and (is evacuated to
0.005MPa, time 3h), it then adds in sodium sulfite and is uniformly mixed, wherein N, N '-methylene-bisacrylamide, persulfuric acid
Ammonium, sodium sulfite mass ratio be respectively 0.2:0.5:1:100, then acquired solution is transferred to the glass mold of nitrogen atmosphere
In, the sodium alginate-acrylamide composite hydrogel is made in insulation reaction 1.5h, i.e. molding at 65 DEG C after sealing.
The taking-up of molding sodium alginate-acrylamide composite hydrogel is cut into homogeneous bulky, with absolute ethyl alcohol and go from
Sub- water was alternately washed every 12 hours, is washed four days, to remove the small molecules such as unreacted acrylamide, is freeze-dried to perseverance
Weight.
By the present embodiment through dry to sodium alginate obtained by constant weight-acrylamide composite hydrogel progress swelling behavior examination
It tests, as a result sees Fig. 2.The result shows that：The swelling ratio of gained hydrogel increases with the increase of pH, and swelling ratio can reach
34.6。
The above results show：Sodium alginate prepared by the present invention-acrylamide composite hydrogel has excellent mechanical property
Energy, heavy metal adsorption and anti-Swelling Capacity.
The foregoing is merely the preferred embodiment of the present invention, it is noted that those of ordinary skill in the art are come
It says, without departing from the concept of the premise of the invention, makes several modifications and variations, these belong to the protection model of the present invention
It encloses.
Claims (9)
1. the preparation method of a kind of sodium alginate-acrylamide composite hydrogel, which is characterized in that it is as follows to specifically include step：
1）Sodium alginate and acrylamide are pressed 1:The mass ratio of (5~12) is soluble in water, obtains uniform mixed liquor I；
2）Crosslinking agent, initiator are added in mixed liquor I successively, addition catalyst obtains mixed liquor after carrying out froth in vacuum processing
II, wherein crosslinking agent, initiator, catalyst and acrylamide mass ratio be (0.05~5):(0.1~2):(0.2~2.5):
100；
3）Gained mixed liquor I I is sealed into the glass mold of protective gas atmosphere, be heated to 40~70 DEG C of insulation reactions 1~
6h is to get the sodium alginate-acrylamide composite hydrogel；
The froth in vacuum treatment conditions are：Pressure is evacuated to as 0.005~0.02MPa, the time is 1~3h.
2. preparation method according to claim 1, which is characterized in that sodium alginate and acrylamide in the mixed liquor I
Total concentration be 10~20wt%.
3. preparation method according to claim 1, which is characterized in that the crosslinking agent is N, N '-methylene bisacrylamide acyl
Amine, N, N'- diallyl tartardiamides, divinylbenzene, multicondensed ethylene glycol diacrylate or multicondensed ethylene glycol diformazan
Base acrylate.
4. preparation method according to claim 1, which is characterized in that the initiator for ammonium persulfate, potassium peroxydisulfate or
Sodium peroxydisulfate.
5. preparation method according to claim 1, which is characterized in that the catalyst is sodium sulfite, sodium hydrogensulfite
Or sodium thiosulfate.
6. preparation method according to claim 1, which is characterized in that step 3）The insulation reaction time for 1.5 ~
2.5h。
7. preparation method according to claim 1, which is characterized in that the protective gas is nitrogen or argon gas.
8. sodium alginate-acrylamide composite hydrogel prepared by any one of claim 1 ~ 7 preparation method.
9. sodium alginate described in claim 8-application of the acrylamide composite hydrogel as the adsorbent of heavy metal ion,
Be characterized in that, for adsorb copper ion, mercury ion, cadmium ion, lead ion, zinc ion, barium ions, chromium ion, manganese ion, cobalt from
Son, nickel ion or tungsten ion.
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