CN107474304A - A kind of graphene oxide sodium alginate magnetic composite and preparation method - Google Patents
A kind of graphene oxide sodium alginate magnetic composite and preparation method Download PDFInfo
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- CN107474304A CN107474304A CN201710836611.3A CN201710836611A CN107474304A CN 107474304 A CN107474304 A CN 107474304A CN 201710836611 A CN201710836611 A CN 201710836611A CN 107474304 A CN107474304 A CN 107474304A
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- sodium alginate
- graphene oxide
- silk
- aqueous solution
- fibroin
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 46
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 46
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229920000962 poly(amidoamine) Polymers 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000003385 sodium Chemical class 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 108010022355 Fibroins Proteins 0.000 claims description 34
- 239000007864 aqueous solution Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 9
- 150000002505 iron Chemical class 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 108090000623 proteins and genes Proteins 0.000 claims description 6
- 102000004169 proteins and genes Human genes 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 238000000502 dialysis Methods 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims 1
- 229920002647 polyamide Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 22
- 239000012620 biological material Substances 0.000 abstract 1
- 239000012567 medical material Substances 0.000 abstract 1
- 238000001338 self-assembly Methods 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 235000018102 proteins Nutrition 0.000 description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000004471 Glycine Substances 0.000 description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 2
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 description 2
- 235000004279 alanine Nutrition 0.000 description 2
- 235000010443 alginic acid Nutrition 0.000 description 2
- 229920000615 alginic acid Polymers 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- 241000255789 Bombyx mori Species 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 241000195474 Sargassum Species 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WQZGKKKJIJFFOK-RWOPYEJCSA-N beta-D-mannose Chemical compound OC[C@H]1O[C@@H](O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-RWOPYEJCSA-N 0.000 description 1
- 229920001222 biopolymer Polymers 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 108010094020 polyglycine Proteins 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009366 sericulture Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 210000002435 tendon Anatomy 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- 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
- C08J9/36—After-treatment
- C08J9/40—Impregnation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
-
- 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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
-
- 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
- C08J2389/00—Characterised by the use of proteins; Derivatives 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
-
- 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
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of graphene oxide sodium alginate magnetic composite and preparation method, preparation process are as follows：Use PAMAM modified sodium alginates；Sodium alginate/silk magnetic porous composite material is obtained using liquid nitrogen, frozen dried；Sodium alginate/silk magnetic porous composite material is immersed in graphene oxide solution, cleaned repeatedly with ethanol and deionized water after taking-up, graphene oxide sodium alginate magnetic composite is obtained after vacuum drying.The present invention uses sodium alginate and silk that graphene oxide is carried out into effective self assembly, graphene oxide sodium alginate magnetic composite is obtained, there is huge application value in fields such as sorbing material, biomaterial, medical materials as base material.
Description
Technical field
The present invention relates to a kind of graphene oxide-sodium alginate magnetic composite, belongs to field of nanocomposite materials.
Background technology
Silk is described as fiber queen, and its is soft, abundant, smooth, plentiful, possesses gloss soft as pearl,
Weaving, apparel industry are widely used.Silk is made up of silk gum and fibroin, and wherein silk gum is located at the outer layer of silk, content
Between 20%-30%, fibroin is located at the internal layer of silk, and content is between 70%-80%.Fibroin positioned at silk internal layer is one
Kind natural macromolecular material, by serine（serine）, glycine（Glycine）, alanine（alanine）Deng 18 kinds of amino
Acid composition, molecular weight is about 2300kDa, is made up of heavy chain, light chain and P25, and wherein the molecular weight of heavy chain H chains is 350kDa, gently
Chain L chain molecular weights are 26kDa, and P25 molecular weight is 30kDa, and the ratio of three is 6:6:1.Fibroin share 11 noncrystalline domains and
12 crystal regions, by disulfide bond between heavy chain H chains and light chain L chains, form H-L complexs.
The crystal habit of fibroin is broadly divided into two kinds of the type of fibroin I and II type of fibroin.The type of fibroin I is a kind of knot of meta-stable
Structure, conformation are crank shape or zigzag, are a kind of intermediatenesses between alpha-helix and beta sheet, and structure cell belongs to orthorhombic
System.Handled through damp and hot, sour, polar solvent etc., the type of fibroin I is easy to change to the type of fibroin II.The type of fibroin II is antiparallel β-folding
Stack structure, belong to orthorhombic system, peptide chain arranged regular, hydrogen bond and intermolecular gravitation make adjacent chain is intersegmental to be tightly combined, tension
It is strong to stretch ability, and is insoluble in water, it is strong to the resistance of acid, alkali, salt, enzyme and heat.In addition, recent years are found that one kind is new again
Fibroin crystal habit, i.e. the type of fibroin III, its crystal structure is similar with polyglycine II, belongs to hexagonal crystal system.
Silk obtained regenerated silk fibroin after degumming, dissolving, purification have nontoxic, non-stimulated, biological degradability,
Biocompatibility, good engineering properties, are easily processed into various forms, as silk protein films, gel, fiber, three-dimensional rack,
Sponge etc., it is a kind of important natural function material, available for fields such as biology, medical science, photoelectric materials, is carried as medicament slow release
Body, tissue engineering bracket, operation suture thread, artificial skin, artificial tendon, cell culture vector, wound dressing, electrically conducting transparent are thin
Film, sorbing material etc.（Silk, 2017,03:6-12；Biomedical engineering magazine, 2015,06:1364-1368；Sericulture section
Learn, 2016,02:341-345）.
With the birth of petroleum base high polymer material, high polymer material extensive use in every field, but its institute's band
The pollution problem come has a strong impact on the living environment of the mankind.And native biopolymer material is with its unique performance and to environment
Close friend, turn into the study hotspot of current new material.Wherein, sodium alginate excellent has biocompatibility, nontoxic as a kind of
And the material of biodegradable, it has been widely used in the fields such as grocery trade, agricultural, medical industry, commodity at present.Sea
Mosanom is also known as algin, sodium alginate or seaweed gel, be extracted from the sea-tangle or sargassum of brown algae iodine and mannitol with
Byproduct afterwards.Sodium alginate is the main component of alginic cell wall and cytoplasm, and marine alga acid molecule is by β-D-MANNOSE
Aldehydic acid（M areas）With α-L- guluronic acids（G areas）The block linear polymer of 2 kinds of monomer compositions.In 1 marine alga acid molecule,
The continuous segment that wherein a kind of uronic acid is formed may be comprised only, it is also possible to form block copolymer by 2 kinds of uronic acid chain links.And
Sodium alginate is the product after alginic acid is neutralized with alkali.Sodium alginate is soluble in water, is the very high poly- electrolysis of a kind of charge density
Matter, there is good biological degradability and compatibility（New Chemical Materials, 2007, (08):20-22）.In sodium alginate structure
Containing substantial amounts of hydroxyl and carboxyl, therefore sodium alginate is the initiation material of an ideal chemistry functional.Pass through
Modification to hydroxyl in structure and carboxyl, its dissolubility, hydrophobicity and some physical and chemical performances is changed, form sea
Mosanom derivation function compound, can widen its application field.At present, the modification for sodium alginate hydroxyl and carboxyl is main
There are oxidation, sulfonation, esterification, amidatioon and graft copolymerization etc.（Huang Panli, Shen Xiaojun, Chen Jinghuan, Wu Yuying, Sun Run storehouse marine algas
The extraction of sour sodium and functional modification progress [J] chemistry of forest product and industry, 2017）.
The existing literature research of sodium alginate/silk fibre composite, but it is mostly film and fiber.Such as Agricultural University Of Anhui's system
For fibroin-sodium alginate-glycerine blend film（Agricultural University Of Anhui's journal, 2013,40 (2): 321-325）, Dalian industry
University utilizes polyethyleneglycol diglycidylether（PEGDE）It is chemically crosslinked fibroin albumen（SF）, with CaCl2Crossslinked sodium alginate
（SA）, SF/SA dual network type composite fibres are prepared for using the method for substep crosslinking（Wish national wealth, Zhang Hong, Li Huitao, Chen Tao, in
Jump, preparation and performance [J] composite journals of the chemical crosslinking modified fibroin albumens of Guo Jing/sodium alginate fiber,
2017）.
2004, Univ Manchester UK physicist An Deliehaimu and Constantine's Nuo Woxiao loves, utilize
The method for tearing adhesive tape, successfully isolates the graphene of individual layer atomic arrangement from graphite, therefore two people also obtain 2010
The Nobel Prize in physics in year（Science,2004,306( 5696):666-669）.Graphene is by carbon atom with sp2Hydridization rail
Road forms hexangle type honeycomb lattice, and its construction unit is carbon hexatomic ring, and it is a kind of two-dimentional material of only single layer of carbon atom thickness
Material.Graphene is the basic system unit for forming carbon-based material.It can be wrapped to form zero dimension Fullerenes, be rolled into one-dimensional
Carbon nanotube, layer upon layer is into three-dimensional graphite.From graphene find that day, graphene just into
For the focus and focus of research, in ultracapacitor, transparency electrode, desalinization, light emitting diode, sensor, hydrogen storage, the sun
The fields such as energy battery, catalyst carrier, composite, biologic bracket material, bio-imaging, drug delivery, weaving, printing and dyeing have extensively
General application（Novel charcoal material, 2014,05:329-356, Chinese invention patent 201410565512.2）.
Graphene composite material is research direction important in graphene application field（Chemical Engineer, 2015,01:34-
38+46）.Existing graphene composite material is by graphene oxide and another material mostly（Inorganic material, polymeric material
Material etc.）Uniformly it is mixed in solvent, finished product is then obtained by the methods of spin processes, vacuum filtration, spin coating.But due to graphene
The problem of certain be present in the π-π stackings effect easily aggregation of itself, its dispersiveness in a solvent（Chemical progress, 2016,05:
647-656）, the preparation of follow-up composite and the final performance of product can be influenceed.
The content of the invention
In view of the above problems, the present invention provides a kind of graphene oxide-sodium alginate magnetic composite and preparation method.
The technical scheme is that：
（1）Sodium alginate is scattered in deionized water under normal temperature, bath raio 1:50, it is slowly added to 1-100g/L polyamide-amide
The PAMAM aqueous solution, the wherein volume ratio of the PAMAM aqueous solution and sodium alginate aqueous solution are 1:1-1:10, after reacting 24h, with steaming
Distilled water and ethanol wash, obtain PAMAM modified sodium alginates after drying repeatedly；（2）Silk-fibroin is dissolved in deionized water, prepared
Into the 1g/L-100g/L aqueous solution, the 1g/L-100g/L trivalent iron salt aqueous solution is slowly dropped under conditions of 50-80 DEG C
In silk protein aqueous solution, stir, wherein the mass ratio of the silk-fibroin and trivalent iron salt is 1:1-10:1,60 DEG C is at the uniform velocity stirred
After mixing 1h, the PAMAM modified sodium alginates that are slowly added in step 1 after ultrasonic mixing is uniform, pour into mould, are put into liquid nitrogen
Middle 1min, pre-freeze 6h in -20 DEG C of refrigerators is placed in after taking-up, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers, is then placed in jelly
48h obtains magnetic porous composite material in dry machine；（3）Configuration concentration 0.1-100g/L graphene oxide water solution, ultrasonic 1h,
Then the magnetic porous composite material in step 2 is immersed in 24h in graphene oxide water solution, bath raio 1:50, used after taking-up
Ethanol and deionized water are cleaned repeatedly, and graphene oxide-sodium alginate magnetic composite is obtained after vacuum drying.
Preferably, the silk-fibroin is that silk is made after degumming, dissolving, dialysis, purification.
Preferably, the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate.
Preferably, the mass ratio of the modified sodium alginate and silk-fibroin is 1:1-1:10.
Compared with prior art, the advantage of the invention is that：PAMAM is polyamidoamine dendrimer, and surface is rich
Containing amino, imido grpup.Using PAMAM modified sodium alginates and silk-fibroin as carrier, firm Covalent bonding together is produced between the two,
Then nano ferriferrous oxide granule is generated, and it is porous compound to obtain after liquid nitrogen, freeze-drying process silk-sodium alginate
Material, final load graphene oxide, it ensure that dispersing uniformity and silkworm of the graphene oxide in silk-sodium alginate matrix
The Stability Analysis of Structures and mechanical strength of silk-sodium alginate porous material.In addition, graphene oxide-sodium alginate magnetic composite
Also there is certain magnetic, it is possible to achieve effective to recycle.
Embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1：
（1）Sodium alginate is scattered in deionized water under normal temperature, bath raio 1:50, it is slowly added to 10g/L polyamide-amide
The PAMAM aqueous solution, the wherein volume ratio of the PAMAM aqueous solution and sodium alginate aqueous solution are 1:1, after reacting 24h, with distilled water and
Ethanol washs, obtains PAMAM modified sodium alginates after drying repeatedly；（2）Silk-fibroin is dissolved in deionized water, is configured to 10g/
The L aqueous solution, 10g/L ferric chloride in aqueous solution is slowly dropped into silk protein aqueous solution under conditions of 50 DEG C, stirring is equal
It is even, wherein the mass ratio of the silk-fibroin and iron chloride is 10:After 1,60 DEG C is at the uniform velocity stirred 1h, it is slowly added in step 1
The mass ratio of PAMAM modified sodium alginates, modified sodium alginate and silk-fibroin is 1:1, after ultrasonic mixing is uniform, pour into mould
In, 1min in liquid nitrogen is put into, pre-freeze 6h in -20 DEG C of refrigerators is placed in after taking-up, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers,
It is then placed in 48h in freeze dryer and obtains magnetic porous composite material；（3）Configuration concentration 10g/L graphene oxide water solution,
Ultrasonic 1h, the magnetic porous composite material in step 2 is then immersed in 24h in graphene oxide water solution, bath raio 1:50,
Cleaned repeatedly with ethanol and deionized water after taking-up, graphene oxide-sodium alginate magnetic composite is obtained after vacuum drying.
Embodiment 2：
（1）Sodium alginate is scattered in deionized water under normal temperature, bath raio 1:50, it is slowly added to 40g/L polyamide-amide
The PAMAM aqueous solution, the wherein volume ratio of the PAMAM aqueous solution and sodium alginate aqueous solution are 1:8, after reacting 24h, with distilled water and
Ethanol washs, obtains PAMAM modified sodium alginates after drying repeatedly；（2）Silk-fibroin is dissolved in deionized water, is configured to 50g/
The L aqueous solution, 50g/L ferric sulfate aqueous solution is slowly dropped into silk protein aqueous solution under conditions of 60 DEG C, stirring is equal
It is even, wherein the mass ratio of the silk-fibroin and ferric sulfate is 1:After 1,60 DEG C is at the uniform velocity stirred 1h, it is slowly added in step 1
The mass ratio of PAMAM modified sodium alginates, modified sodium alginate and silk-fibroin is 1:4, after ultrasonic mixing is uniform, pour into mould
In, 1min in liquid nitrogen is put into, pre-freeze 6h in -20 DEG C of refrigerators is placed in after taking-up, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers,
It is then placed in 48h in freeze dryer and obtains magnetic porous composite material；（3）Configuration concentration 50g/L graphene oxide water solution,
Ultrasonic 1h, the magnetic porous composite material in step 2 is then immersed in 24h in graphene oxide water solution, bath raio 1:50,
Cleaned repeatedly with ethanol and deionized water after taking-up, graphene oxide-sodium alginate magnetic composite is obtained after vacuum drying.
Embodiment 3：
（1）Sodium alginate is scattered in deionized water under normal temperature, bath raio 1:50, it is slowly added to 100g/L polyamide-amide
The PAMAM aqueous solution, the wherein volume ratio of the PAMAM aqueous solution and sodium alginate aqueous solution are 1:10, after reacting 24h, use distilled water
Washed repeatedly with ethanol, obtain PAMAM modified sodium alginates after drying；（2）Silk-fibroin is dissolved in deionized water, is configured to
The 50g/L aqueous solution, 50g/L iron nitrate aqueous solution is slowly dropped into silk protein aqueous solution under conditions of 80 DEG C, stirred
Uniformly, wherein the mass ratio of the silk-fibroin and ferric nitrate is 2:After 1,60 DEG C is at the uniform velocity stirred 1h, it is slowly added in step 1
The mass ratio of PAMAM modified sodium alginates, modified sodium alginate and silk-fibroin is 1:9, after ultrasonic mixing is uniform, pour into mould
In, 1min in liquid nitrogen is put into, pre-freeze 6h in -20 DEG C of refrigerators is placed in after taking-up, 6h is freezed in -80 DEG C of Thermo ultra low temperature freezers,
It is then placed in 48h in freeze dryer and obtains magnetic porous composite material；（3）Configuration concentration 100g/L graphene oxide is water-soluble
Liquid, ultrasonic 1h, the magnetic porous composite material in step 2 is then immersed in 24h in graphene oxide water solution, bath raio 1:
50, cleaned repeatedly with ethanol and deionized water after taking-up, graphene oxide-sodium alginate magnetic coupling material is obtained after vacuum drying
Material.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is amplified out still in protection scope of the present invention.
Claims (5)
- A kind of 1. preparation method of graphene oxide-sodium alginate magnetic composite, it is characterised in that：Step 1：Sodium alginate is scattered in deionized water under normal temperature, bath raio 1:50, it is slowly added to 1-100g/L polyamides Amine-amine PAMAM the aqueous solution, the wherein volume ratio of the PAMAM aqueous solution and sodium alginate aqueous solution are 1:1-1:10, after reacting 24h, Washed repeatedly with distilled water and ethanol, obtain PAMAM modified sodium alginates after drying；Step 2：Silk-fibroin is dissolved in deionized water, is configured to the 1g/L-100g/L aqueous solution, will under conditions of 50-80 DEG C The 1g/L-100g/L trivalent iron salt aqueous solution is slowly dropped into silk protein aqueous solution, is stirred, wherein the silk-fibroin Mass ratio with trivalent iron salt is 1:1-10:After 1,60 DEG C is at the uniform velocity stirred 1h, the PAMAM being slowly added in step 1 is modified marine alga Sour sodium, after ultrasonic mixing is uniform, pour into mould, be put into 1min in liquid nitrogen, be placed in pre-freeze 6h in -20 DEG C of refrigerators after taking-up, -80 6h is freezed in DEG C Thermo ultra low temperature freezers, 48h in freeze dryer is then placed in and obtains magnetic porous composite material；Step 3：Configuration concentration 0.1-100g/L graphene oxide water solution, ultrasonic 1h are then more by the magnetic in step 2 Hole composite material is immersed in 24h in graphene oxide water solution, bath raio 1:50, it is repeatedly clear with ethanol and deionized water after taking-up Wash, graphene oxide-sodium alginate magnetic composite is obtained after vacuum drying.
- 2. a kind of preparation method of graphene oxide-sodium alginate magnetic composite according to claim 1, its feature It is, the silk-fibroin is that silk is made after degumming, dissolving, dialysis, purification.
- 3. a kind of preparation method of graphene oxide-sodium alginate magnetic composite according to claim 1, its feature It is, the trivalent iron salt is the one or more in iron chloride, ferric sulfate, ferric nitrate.
- 4. a kind of preparation method of graphene oxide-sodium alginate magnetic composite according to claim 1, its feature It is, the mass ratio of the modified sodium alginate and silk-fibroin is 1:1-1:10.
- A kind of 5. graphene oxide-sodium alginate magnetic composite obtained by claim 1 preparation method.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109851389A (en) * | 2019-01-12 | 2019-06-07 | 马小良 | A kind of preparation method of magnetic porous ceramics |
| CN112266497A (en) * | 2020-11-04 | 2021-01-26 | 北京航空航天大学 | A kind of shell-like lightweight high-strength composite material and preparation method thereof |
| CN113952936A (en) * | 2021-10-13 | 2022-01-21 | 天津工业大学 | Polyamide-amine modified sodium alginate gel ball for removing heavy metal ions in water and preparation method thereof |
| CN115341306A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | Graphene aerogel fiber and preparation method thereof |
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| CN103572395A (en) * | 2013-11-14 | 2014-02-12 | 东华大学 | Strengthened toughened regenerated silk fibers and preparation method thereof |
| CN106117570A (en) * | 2016-06-24 | 2016-11-16 | 武汉理工大学 | A kind of sodium alginate anti-bacterial hydrogel loading daiamid dendrimer and its preparation method and application |
| CN106830096A (en) * | 2017-02-28 | 2017-06-13 | 东南大学 | A kind of preparation method of magnetic Nano iron oxide |
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| CN103572395A (en) * | 2013-11-14 | 2014-02-12 | 东华大学 | Strengthened toughened regenerated silk fibers and preparation method thereof |
| CN106117570A (en) * | 2016-06-24 | 2016-11-16 | 武汉理工大学 | A kind of sodium alginate anti-bacterial hydrogel loading daiamid dendrimer and its preparation method and application |
| CN106830096A (en) * | 2017-02-28 | 2017-06-13 | 东南大学 | A kind of preparation method of magnetic Nano iron oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109851389A (en) * | 2019-01-12 | 2019-06-07 | 马小良 | A kind of preparation method of magnetic porous ceramics |
| CN112266497A (en) * | 2020-11-04 | 2021-01-26 | 北京航空航天大学 | A kind of shell-like lightweight high-strength composite material and preparation method thereof |
| CN112266497B (en) * | 2020-11-04 | 2021-09-14 | 北京航空航天大学 | Shell-like light high-strength composite material and preparation method thereof |
| CN113952936A (en) * | 2021-10-13 | 2022-01-21 | 天津工业大学 | Polyamide-amine modified sodium alginate gel ball for removing heavy metal ions in water and preparation method thereof |
| CN115341306A (en) * | 2022-09-23 | 2022-11-15 | 内蒙古大学 | Graphene aerogel fiber and preparation method thereof |
| CN115341306B (en) * | 2022-09-23 | 2023-04-28 | 内蒙古大学 | A kind of graphene airgel fiber and preparation method thereof |
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