CN109232815A - A kind of preparation method and applications of acrylic acid complex polysaccharide class hydrogel - Google Patents
A kind of preparation method and applications of acrylic acid complex polysaccharide class hydrogel Download PDFInfo
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- CN109232815A CN109232815A CN201810804658.6A CN201810804658A CN109232815A CN 109232815 A CN109232815 A CN 109232815A CN 201810804658 A CN201810804658 A CN 201810804658A CN 109232815 A CN109232815 A CN 109232815A
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 49
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000000017 hydrogel Substances 0.000 title claims abstract description 40
- 150000004676 glycans Chemical class 0.000 title claims abstract description 25
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 25
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 229920001661 Chitosan Polymers 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000005457 ice water Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 229920002307 Dextran Polymers 0.000 claims abstract description 7
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 46
- 229920001503 Glucan Polymers 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 238000004090 dissolution Methods 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 claims description 2
- 239000010865 sewage Substances 0.000 claims description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229940058573 b-d glucose Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/36—Amides or imides
- C08F222/38—Amides
- C08F222/385—Monomers containing two or more (meth)acrylamide groups, e.g. N,N'-methylenebisacrylamide
-
- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Medicinal Preparation (AREA)
Abstract
本发明属于高分子复合材料技术领域，涉及水凝胶的制备，尤其涉及丙烯酸复合多糖类水凝胶的制备方法。包括：按照每5 mL去离子水溶解氢氧化钠，再等比例量取5 mL丙烯酸，在冰水浴中滴加丙烯酸中和，中和度达到65～80%后，得到溶液A；按照每10 mL去离子水超声溶解壳聚糖和葡聚糖，配成0.1～1.6wt%壳聚糖和1～4wt%葡聚糖溶液，得到溶液B；将溶液B倒入溶液A中混合得到溶液C，加入引发剂搅拌均匀，再加交联剂溶解，65～85℃超声3～4h后，得到水凝胶粗样；用无水乙醇浸泡粗样10 h，60℃下真空干燥24 h，研磨成粉，干燥即得。本发明所述方法简单绿色环保、易于操作、成本低廉，没有产生大量的污染环境的废水。所制备的水凝胶的性能良好，适合工业化生产。
The invention belongs to the technical field of polymer composite materials, and relates to the preparation of hydrogels, in particular to a preparation method of acrylic acid composite polysaccharide hydrogels. Including: dissolve sodium hydroxide per 5 mL of deionized water, then measure 5 mL of acrylic acid in equal proportions, add acrylic acid dropwise in an ice-water bath for neutralization, and obtain solution A after the degree of neutralization reaches 65-80%; mL deionized water ultrasonically dissolves chitosan and dextran, and prepares a solution of 0.1-1.6wt% chitosan and 1-4wt% dextran to obtain solution B; solution B is poured into solution A and mixed to obtain solution C , add the initiator and stir evenly, then add the cross-linking agent to dissolve, after sonicating at 65-85 ℃ for 3-4 h, a crude hydrogel sample is obtained; soak the crude sample in absolute ethanol for 10 h, vacuum dry at 60 ℃ for 24 h, grind Powder and dry. The method of the invention is simple, environmentally friendly, easy to operate, low in cost, and does not generate a large amount of waste water that pollutes the environment. The prepared hydrogel has good performance and is suitable for industrial production.
Description
Technical field
The invention belongs to technical field of polymer composite materials, be related to hydrogel preparation more particularly to a kind of acrylic acid
The preparation method and applications of complex polysaccharide class hydrogel.
Background technique
Chitosan (chitosan) is also known as chitosan, is chitin (chitin) warp being widely present by nature
Cross what deacetylation obtained, chemical name is Chitosan (1-4) -2- amino-B-D glucose.From Frenchman in 1859
After Rouget obtains chitosan first, the biological functionality and compatibility of this natural polymer, blood compatibility, safety,
The excellent performances such as microbic resolvability are by all trades and professions extensive concern, in medicine, food, chemical industry, cosmetics, water process, metal
It extracts and the application study of the numerous areas such as recycling, biochemical and biomedical engineering achieves major progress.Chitosan is that have
Polyhydroxy-OH, polyamino-NH2The high-molecular compound of structure, this make it application it is very extensive, can occur aoxidize, be alkylated,
The reaction such as graft copolymerization, esterification, condensation, sulfonation.
Glucan (dextran) is the oligomeric polysaccharide formed by multiple glucose polycondensations, has single glucose all
Advantage possesses more active function groups since it is polymer, this keeps it more active in chemical reaction, can occur more
Kind reaction, e.g., esterification, hydrolysis, sulfonation, alkylation, graft copolymerization etc..Glucan has good biocompatibility, in medical treatment
Aspect is widely used.
In conclusion acrylic acid and two kinds of polysaccharide composites form hydrogel, itself item of hydrogel can be greatly improved
Performance, more hydrophilic radical increase substantially hydrogel water retention property can, and polysaccharide provides more functional groups, make
It is more superior in the performance of the applications such as adsorption treatment heavy metal ion, dyestuff, ammonia.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is be anti-with acrylic acid, chitosan, glucan
Monomer is answered, initiator and crosslinking agent is added, utilizes the method synthetic hydrogel of ultrasonic wave added.
Technical scheme is as follows:
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
A, 5 mL acrylic acid are measured according to every 5 mL deionized water dissolving, 1.8980~2.3360 g sodium hydroxide, then equal proportion,
In ice-water bath be added dropwise acrylic acid in and sodium hydroxide, after degree of neutralization reaches 65~80%, obtain solution A；
B, according to every 10 mL deionized water ultrasonic dissolution chitosan and glucan, be made into 0.1~1.6wt% chitosan and 1~
4wt% dextran solution, obtains solution B；
C, solution B is poured into be uniformly mixed in solution A and obtains solution C, initiator is first added and stirs evenly, adds crosslinking agent
Stirring and dissolving after 65~85 DEG C of 3~4h of ultrasound, obtains hydrogel study；
D, with 10 h of soaked in absolute ethyl alcohol study, 24 h then is dried in vacuo at 60 DEG C, are pulverized, kept dry.
In the more excellent disclosed example of the present invention, every 5 mL deionized water dissolving, 2.3360 g sodium hydroxide described in step A.
In the more excellent disclosed example of the present invention, it is added dropwise in acrylic acid in ice-water bath described in step A and is reached with sodium hydroxide, degree of neutralization
To 80%.
In the more excellent disclosed example of the present invention, every 10 mL deionized water ultrasonic dissolution chitosan and glucan, match described in step B
At 1wt% chitosan and 3wt% dextran solution.
In the more excellent disclosed example of the present invention, initiator described in step C is potassium peroxydisulfate, and additive amount is mixed solution total weight
0.4~0.8wt%；The crosslinking agent be N ' N- methylene-bisacrylamide, additive amount be mixed solution total weight 0.04~
0.08wt%。
In the more excellent disclosed example of the present invention, initiator potassium persulfate additive amount described in step C is mixed solution total weight
0.5wt%；Crosslinking agent N ' the N- methylene-bisacrylamide additive amount is the 0.05wt% of mixed solution total weight.
Acrylic acid complex polysaccharide class hydrogel made from the method according to the present invention, surface have a large amount of ducts, also
Many folds.
Another object of the present invention, be by obtained acrylic acid complex polysaccharide class hydrogel be used as adsorbent with
Heavy-metal ion removal, dyestuff, ammonia etc. carry out sewage treatment.
Agents useful for same of the present invention is all that analysis is pure, is commercially available.
Beneficial effect
The present invention makes acrylic acid, chitosan, glucan be copolymerized to form hydrogel in the method for ultrasonic wave added.Institute of the present invention
It states simple environmentally protective, the easily operated, raw material of process flow and is easy to get low in cost, while also achieving the green of synthesis technology
Change, does not generate the waste water of a large amount of pollution environment.Functional, the suitable industrialized production of prepared hydrogel.
Detailed description of the invention
The infrared figure of acrylic acid complex polysaccharide class hydrogel obtained by Fig. 1 embodiment of the present invention 2；
The scanning electron microscope (SEM) photograph of acrylic acid complex polysaccharide class hydrogel obtained by Fig. 2 embodiment of the present invention 2.
Specific embodiment
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Embodiment 1
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
1.8980 g NaOH are weighed in the beaker of 50 mL, 5 mL deionized water dissolvings are added, then weigh 5 mL acrylic acid,
It places the beaker in ice-water bath, draws acrylic acid with dropper and be added drop-wise in NaOH, stirred when being added dropwise, until the acrylic acid of 5 mL
It is all added drop-wise in beaker, stands at room temperature, obtain solution A；It weighs 0.01 g chitosan respectively again and 0.1 g glucan adds
Enter in 50 mL beakers, the deionized water for measuring 10 mL is added in beaker, and beaker is then placed on ultrasonic dissolution in Ultrasound Instrument, is obtained
To solution B；Solution B is poured into solution A, with glass bar stirring and dissolving；0.16 g potassium peroxydisulfate is weighed again, and solution C is added
In, with glass bar stirring and dissolving；Then it weighs 0.0085 g N ' N- methylene-bisacrylamide to be added in solution C, stir molten
Solution, places the beaker 3 h of ultrasound at 65 DEG C, obtains study after to be dissolved；10 h of soaked in absolute ethyl alcohol is used again, then puts sample
It is dried in vacuo 24 h in 60 DEG C of baking oven, finally grinds to obtain powder, is placed in drier and saves.
Synthesized hydrogel is for when adsorbing heavy metal ion, adsorbent additive amount to be 0.01 g, Cu2+Adsorbance is
342 mg· g-1, Co2+For 232 mg g-1, Ni2+For 185 mg g-1, Pb2+For 395 mg g-1, Cd2+It is 269
mg·g-1 。
Embodiment 2
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
2.3360 g NaOH are weighed in the beaker of 50 mL, 5 mL deionized water dissolvings are added, then weigh 5 mL acrylic acid,
It places the beaker in ice-water bath, draws acrylic acid with dropper and be added drop-wise in NaOH, stirred when being added dropwise, until the acrylic acid of 5 mL
It is all added drop-wise in beaker, stands at room temperature, obtain solution A；It weighs 0.11 g chitosan respectively again and 0.1 g glucan adds
Enter in 50 mL beakers, the deionized water for measuring 10 mL is added in beaker, and beaker is then placed on ultrasonic dissolution in Ultrasound Instrument, is obtained
To solution B；Solution B is poured into solution A, with glass bar stirring and dissolving；0.07g potassium peroxydisulfate is weighed again to be added in solution C,
With glass bar stirring and dissolving；Then it weighs 0.0115 g N ' N- methylene-bisacrylamide to be added in solution C, stirring and dissolving,
3 h of ultrasound at 65 DEG C are placed the beaker after to be dissolved, obtain study；10 h of soaked in absolute ethyl alcohol is used again, is then placed on sample
It is dried in vacuo 24 h in 60 DEG C of baking oven, finally grinds to obtain powder, is placed in drier and saves.
In Fig. 1,3416 cm-1It is poly- to belong to shell by the stretching vibration peak for belonging to-the OH ,-OH in chitosan molecule
The characteristic peak of sugar；2936 cm-1Belong to-CH2Stretching vibration peak；1673 cm-1For C=O stretching vibration peak, belong to amide groups
C=O stretching vibration peak in C=O stretching vibration peak and acrylic acid carboxylic group in group；1556 cm-1Belong to-NH2Deformation vibration
Dynamic peak, 1408 cm-1- OH deformation vibration peak is belonged to, the peak C-N is in 1319 cm-1Near, C-O stretching vibration peak is in 1168 cm-1
Left and right, 1047 cm-1Belong to C-O-C stretching vibration peak, 782 cm-1For the peak of c h bond.
In Fig. 2, hydrogel surface has a large amount of ducts, and there are many more folds.
Synthesized hydrogel is for when adsorbing heavy metal ion, adsorbent additive amount to be 0.01 g, Cu2+Adsorbance is
322 mg· g-1, Co2+For 202 mg g-1, Ni2+For 195 mg g-1, Pb2+For 325 mg g-1, Cd2+It is 249
mg· g-1 。
Embodiment 3
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
1.9600 g NaOH are weighed in the beaker of 50 mL, 5 mL deionized water dissolvings are added, then weigh 5 mL acrylic acid,
It places the beaker in ice-water bath, draws acrylic acid with dropper and be added drop-wise in NaOH, stirred when being added dropwise, until the acrylic acid of 5 mL
It is all added drop-wise in beaker, stands at room temperature, obtain solution A；It weighs 0.06 g chitosan respectively again and 0.2 g glucan adds
Enter in 50 mL beakers, the deionized water for measuring 10 mL is added in beaker, and beaker is then placed on ultrasonic dissolution in Ultrasound Instrument, is obtained
To solution B；Solution B is poured into solution A, with glass bar stirring and dissolving；0.11g potassium peroxydisulfate is weighed again to be added in solution C,
With glass bar stirring and dissolving；Then it weighs 0.0175 g N ' N- methylene-bisacrylamide to be added in solution C, stirring and dissolving,
3 h of ultrasound at 85 DEG C are placed the beaker after to be dissolved, obtain study；10 h of soaked in absolute ethyl alcohol is used again, is then placed on sample
It is dried in vacuo 24 h in 60 DEG C of baking oven, finally grinds to obtain powder, is placed in drier and saves.
Synthesized hydrogel is for when adsorbing heavy metal ion, adsorbent additive amount to be 0.01 g, Cu2+Adsorbance is
352 mg· g-1, Co2+For 242 mg g-1, Ni2+For 165 mg g-1, Pb2+For 385 mg g-1, Cd2+It is 259
mg· g-1 。
Embodiment 4
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
2.1900 g NaOH are weighed in the beaker of 50 mL, 5 mL deionized water dissolvings are added, then weigh 5 mL acrylic acid,
It places the beaker in ice-water bath, draws acrylic acid with dropper and be added drop-wise in NaOH, stirred when being added dropwise, until the acrylic acid of 5 mL
It is all added drop-wise in beaker, stands at room temperature, obtain solution A；It weighs 0.16 g chitosan respectively again and 0.3 g glucan adds
Enter in 50 mL beakers, the deionized water for measuring 10 mL is added in beaker, and beaker is then placed on ultrasonic dissolution in Ultrasound Instrument, is obtained
To solution B；Solution B is poured into solution A, with glass bar stirring and dissolving；0.13g potassium peroxydisulfate is weighed again to be added in solution C,
With glass bar stirring and dissolving；Then it weighs 0.0145 g N ' N- methylene-bisacrylamide to be added in solution C, stirring and dissolving,
3 h of ultrasound at 65 DEG C are placed the beaker after to be dissolved, obtain study；10 h of soaked in absolute ethyl alcohol is used again, is then placed on sample
It is dried in vacuo 24 h in 60 DEG C of baking oven, finally grinds to obtain powder, is placed in drier and saves.
Synthesized hydrogel is for when adsorbing heavy metal ion, adsorbent additive amount to be 0.01 g, Cu2+Adsorbance is
342 mg· g-1, Co2+For 242 mg g-1, Ni2+For 195 mg g-1, Pb2+For 365 mg g-1, Cd2+It is 259
mg· g-1 。
Embodiment 5
A kind of preparation method of acrylic acid complex polysaccharide class hydrogel, includes the following steps:
2.0440 g NaOH are weighed in the beaker of 50 mL, 5 mL deionized water dissolvings are added, then weigh 5 mL acrylic acid,
It places the beaker in ice-water bath, draws acrylic acid with dropper and be added drop-wise in NaOH, stirred when being added dropwise, until the acrylic acid of 5 mL
It is all added drop-wise in beaker, stands at room temperature, obtain solution A；It weighs 0.16 g chitosan respectively again and 0.4 g glucan adds
Enter in 50 mL beakers, the deionized water for measuring 10 mL is added in beaker, and beaker is then placed on ultrasonic dissolution in Ultrasound Instrument, is obtained
To solution B；Solution B is poured into solution A, with glass bar stirring and dissolving；0.09 g potassium peroxydisulfate is weighed again, and solution C is added
In, with glass bar stirring and dissolving；Then it weighs 0.0175 g N ' N- methylene-bisacrylamide to be added in solution C, stir molten
Solution, places the beaker 3 h of ultrasound at 75 DEG C, obtains study after to be dissolved；10 h of soaked in absolute ethyl alcohol is used again, then puts sample
It is dried in vacuo 24 h in 60 DEG C of baking oven, finally grinds to obtain powder, is placed in drier and saves.
Synthesized hydrogel is for when adsorbing heavy metal ion, adsorbent additive amount to be 0.01 g, Cu2+Adsorbance is
322 mg· g-1, Co2+For 212 mg g-1, Ni2+For 175 mg g-1, Pb2+For 355 mg g-1, Cd2+It is 255
mg· g-1 。
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of acrylic acid complex polysaccharide class hydrogel, which comprises the steps of:
5 mL acrylic acid are measured according to every 5 mL deionized water dissolving, 1.8980~2.3360 g sodium hydroxide, then equal proportion,
In ice-water bath be added dropwise acrylic acid in and sodium hydroxide, after degree of neutralization reaches 65~80%, obtain solution A；
According to every 10 mL deionized water ultrasonic dissolution chitosan and glucan, it is made into 0.1~1.6wt% chitosan and 1~4wt%
Dextran solution obtains solution B；
Solution B is poured into be uniformly mixed in solution A and obtains solution C, initiator is first added and stirs evenly, adds crosslinking agent stirring
It dissolves, after 65~85 DEG C of 3~4h of ultrasound, obtains hydrogel study；
With 10 h of soaked in absolute ethyl alcohol study, 24 h then are dried in vacuo at 60 DEG C, are pulverized, kept dry.
2. the preparation method of acrylic acid complex polysaccharide class hydrogel according to claim 1, it is characterised in that: described in step A
Every 5 mL deionized water dissolving, 2.3360 g sodium hydroxide.
3. the preparation method of acrylic acid complex polysaccharide class hydrogel according to claim 1, it is characterised in that: described in step A
It is added dropwise in ice-water bath in acrylic acid and sodium hydroxide, degree of neutralization reaches 80%.
4. the preparation method of acrylic acid complex polysaccharide class hydrogel according to claim 1, it is characterised in that: described in step B
Every 10 mL deionized water ultrasonic dissolution chitosan and glucan, are made into 1wt% chitosan and 3wt% dextran solution.
5. the preparation method of acrylic acid complex polysaccharide class hydrogel according to claim 1, it is characterised in that: described in step C
Initiator is potassium peroxydisulfate, and additive amount is 0.4~0.8wt% of mixed solution total weight；The crosslinking agent is N ' N- di-2-ethylhexylphosphine oxide
Acrylamide, additive amount are 0.04~0.08wt% of mixed solution total weight.
6. the preparation method of acrylic acid complex polysaccharide class hydrogel according to claim 5, it is characterised in that: described in step C
Initiator potassium persulfate additive amount is the 0.5wt% of mixed solution total weight；Crosslinking agent N ' the N- methylene-bisacrylamide adds
Dosage is the 0.05wt% of mixed solution total weight.
7. acrylic acid complex polysaccharide class hydrogel made from -6 any the methods according to claim 1, it is characterised in that: surface
With a large amount of ducts, there are many more folds.
8. the application of acrylic acid complex polysaccharide class hydrogel described in a kind of claim 7, it is characterised in that: be used as adsorbent
Carry out sewage treatment.
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