CN107337764A - The preparation method and application of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group - Google Patents
The preparation method and application of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group Download PDFInfo
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- CN107337764A CN107337764A CN201710425338.5A CN201710425338A CN107337764A CN 107337764 A CN107337764 A CN 107337764A CN 201710425338 A CN201710425338 A CN 201710425338A CN 107337764 A CN107337764 A CN 107337764A
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- China
- Prior art keywords
- wheat
- rice
- hemicellulose
- corn stalk
- stalks
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Links
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 99
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 79
- 241000209140 Triticum Species 0.000 title claims abstract description 79
- 235000021307 Triticum Nutrition 0.000 title claims abstract description 79
- 235000009566 rice Nutrition 0.000 title claims abstract description 79
- 240000008042 Zea mays Species 0.000 title claims abstract description 75
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 75
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 63
- 235000005822 corn Nutrition 0.000 title claims abstract description 63
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 240000007594 Oryza sativa Species 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000010902 straw Substances 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 238000001179 sorption measurement Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 16
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 claims abstract description 12
- 235000009973 maize Nutrition 0.000 claims abstract description 12
- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical class CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000004132 cross linking Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 241000209094 Oryza Species 0.000 claims description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- -1 disulfobenzene sodium sulfonates Chemical class 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 238000012545 processing Methods 0.000 claims description 15
- 239000000178 monomer Substances 0.000 claims description 13
- 235000005305 Nypa fruticans Nutrition 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 8
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 8
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 230000001186 cumulative effect Effects 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 244000004005 Nypa fruticans Species 0.000 claims 3
- 241000255964 Pieridae Species 0.000 claims 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims 1
- 235000011130 ammonium sulphate Nutrition 0.000 claims 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims 1
- 239000000499 gel Substances 0.000 abstract description 70
- 239000000017 hydrogel Substances 0.000 abstract description 13
- GGMPTLAAIUQMIE-UHFFFAOYSA-N 2,3,4,5,6-pentachlorobiphenyl Chemical group ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1C1=CC=CC=C1 GGMPTLAAIUQMIE-UHFFFAOYSA-N 0.000 abstract description 11
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachlorophenol Chemical compound OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 abstract description 10
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- 210000000780 bap Anatomy 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000003809 water extraction Methods 0.000 abstract description 3
- 238000003795 desorption Methods 0.000 abstract description 2
- FIKFOOMAUXPBJM-UHFFFAOYSA-N hepta-2,5-dienediamide Chemical class NC(=O)C=CCC=CC(N)=O FIKFOOMAUXPBJM-UHFFFAOYSA-N 0.000 abstract 1
- 101001024118 Homo sapiens Nuclear-interacting partner of ALK Proteins 0.000 description 9
- 102100035376 Nuclear-interacting partner of ALK Human genes 0.000 description 9
- 241000233803 Nypa Species 0.000 description 9
- 238000007605 air drying Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000003344 environmental pollutant Substances 0.000 description 7
- 231100000719 pollutant Toxicity 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 230000003716 rejuvenation Effects 0.000 description 3
- 238000009418 renovation Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 2
- 238000011001 backwashing Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229920000578 graft copolymer Polymers 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000013520 petroleum-based product Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- 229920001221 xylan Polymers 0.000 description 2
- 150000004823 xylans Chemical class 0.000 description 2
- YICILWNDMQTUIY-UHFFFAOYSA-N 2-methylidenepentanamide Chemical compound CCCC(=C)C(N)=O YICILWNDMQTUIY-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010064571 Gene mutation Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000018729 macromolecule modification Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- CHDKQNHKDMEASZ-UHFFFAOYSA-N n-prop-2-enoylprop-2-enamide Chemical class C=CC(=O)NC(=O)C=C CHDKQNHKDMEASZ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 230000036642 wellbeing Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0057—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
Abstract
The present invention discloses a kind of preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group, this method removes the peel air-dried maize straw, grind and screening obtains acceptable material, hemicellulose in hot-water extraction technology separation acceptable material is assisted using alkali, then aqueous solution micellar copolymerization method is passed through, by N N-isopropylacrylamides and phenyl methacrylate graft copolymerization on hemicellulose macromolecular chain, and and N, N methylene-bisacrylamides carry out cross-linking reaction, obtain hydrophobicity corn stalk stalks of rice, wheat, etc. hemicellulose group temperature-sensitive hydrogel；The obtained white bulk of gel, to pentachlorophenol, pentachlorodiphenyl and 3,4 BaPs have higher adsorption capacity, pass through temperature control absorption and desorption, the gel is reusable without losing adsorption, belongs to environmentally friendly hydrophobic organic pollution temperature control sorbing material.
Description
Technical field
The present invention relates to a kind of hemicellulose graft copolymerization hydrophobically modified based on the corn stalk stalks of rice, wheat, etc. to prepare thermo-sensitive gel, is used for
The adsorption treatment of hydrophobic organic pollutant, belong to natural macromolecule modification field of material technology.
Background technology
With the fast development of China's chemical industry, substantial amounts of industrial wastewater especially persistence organic pollutant, without
Processing is discharged directly into water body, causes water environment pollution problem getting worse, significant damage is also resulted in health.
Many organic pollutions, such as polycyclic aromatic hydrocarbon, aromatic compound, Polychlorinated biphenyls etc., there are hydrophobicity, therefore these pollutants
Also referred to as hydrophobic organic pollutant（HOCs）.HOCs is most to be had carcinogenic, teratogenesis, causes gene mutation effect, can be in biology
Cylinder accumulation, health threat finally is caused to animal and human body.By years of researches, it is believed that processing HOCs is more effective
One of means be adsorption technology, i.e., HOCs is separated from water body using sorbing material, then its concentrate is taken into height
The multistage such as level oxidation or burning carries out harmless treatment.However, absorption method applied in reagent present in because HOCs is water-soluble
Difference and concentration is low causes the rate of adsorption slow, adsorbent reactivation difficulty causes financial cost high and secondary pollution problems limitation occurs
Its scale application.Therefore, according to the above-mentioned characteristics of HOCs in waste water, the sorbing material of selection efficiently, economic actual answers it
Processing for HOCs seems most important.
In recent years, substantial amounts of research shows that intelligent temperature-sensitive hydrogel is a kind of excellent water treatment absorbent material, this master
If due to its pollutant is adsorbed it is especially fast, when hydrogel after waste water with being swelled, and then quickly formation gel-water termination
On concentration gradient, pollutant the active force such as hydration and hydrogen bond drive lower pollutant from solution to gel surface spread
And it is adsorbed；Its another big advantage is that regeneration is easy, change liquidus temperature above or below gel critical-temperature when, hydrogen bond etc.
Active force reduces, and polymer chain, which retracts into, causes hydrone and pollutant to be extruded, and realizes the regeneration of hydrogel adsorbent.Temperature
In terms of absorption of the quick hydrogel to pollutant is concentrated mainly on the hydrophily such as heavy metal, dyestuff pollutant process at present.It is but temperature sensitive
Hydrogel will can realize that effective absorption to hydrophobic organic pollutant must just introduce hydrophobic grouping in hydrogel network,
Gel surface is changed into hydrophobic property by hydrophily, the Adsorption to HOCs is realized and improved by heat resistance and salt tolerance.
At present, most of hydrogels are prepared by petroleum-based products, and these hydrogels are not only difficult to degrade, pollute ring
Border, and its source is non-renewable, therefore, water is prepared using agricultural-forestry biomass resource part even replacing whole petroleum-based products
Gel is imperative.In nature, hemicellulose level very abundant, the content especially in grass is up to 1/
3 and more than, be only second to content of cellulose.Hemicellulose is the heterogeneity glycan being made up of different glycan bases, is contained in molecular weight
Substantial amounts of reactive hydroxyl, can be esterified, be etherified, graft copolymerization etc. it is modified, so as to prepare hemicellulose group function material
Material.Wherein, the application study of hemicellulose group gel in the treatment of waste water is of common occurrence.By acrylic graft copolymer in xylan
Class hemicellulose prepares xylan-g- acrylic hydrogels, the Pd in the adsorbable aqueous solution2+、Cd2+, Zn2+Etc. heavy metal ion,
And there is good power of regeneration and heavy metal removal rate, the energy of adsorption of heavy metal ion is not interfered with during recycling yet
Power.The Organic-inorganic composite hydrogel prepared using hemicellulose and multi-walled carbon nanotube, also show good methylene
Blue absorption property.In redox ammonium persulfate/tetramethylethylenediamine system, with N, N- diacrylamines are crosslinking agent, will
Xylan class hemicellulose and acrylic graft copolymer, which prepare hydrogel, has good swelling behavior, and to pH, ion and has
Solvent has good response.To sum up analyze, as a kind of environmentally friendly water treatment absorbent, develop based on HOCs's
It is feasible effectively to remove the temperature-sensitive hydrogel of the hemicellulose group hydrophobically modified of research, and has highly important economic benefit
And social benefit.
China is corn planting big country, and maize straw yield up to 2.2 hundred million tons, in rural area remove by this huge living resources
Be used as outside domestic energy, largely abandon in ground, or on-site incineration.How this kind of agricultural wastes performance self-value is used
Promote the well-being of mankind turns into the important topic studied now.At present, corn stalk skin is as fibrous raw material in pulp and paper industry
In applied, alleviate the severe situation of China Papermaking Resource shortage.However, the corn stalk stalks of rice, wheat, etc.（Also known as cornstalk core）Due to
Form the non-fiber cell that cell is mostly short and small, wall is thin, frangible（Or it is heteroproteose cell）, the application in fiber industry receives
Serious limitation, considerably reduce the application value of maize straw.Although the small part stalk stalks of rice, wheat, etc. is had been developed that as feed manufacturing
Or alcoholic fermentation industry, but restricted by own characteristic and transformation technology, there is no large-scale commercial Application also now.But no
Deniable to be, containing abundant hemicellulose macromolecule in the corn stalk stalks of rice, wheat, etc., lignin content is relatively low, and the cell membrane of the cornstalk stalks of rice, wheat, etc.
Short texture, reaction specific surface area is big, is advantageous to the separation and extraction of high molecular component, therefore, from raw material components and structure
Prove the initial feed that the corn stalk stalks of rice, wheat, etc. can extract as hemicellulose.
The pollution problem of water body hydrophobic organic with reference to caused by modern industry, the application are described in detail using the corn stalk stalks of rice, wheat, etc. as raw material
The technological process of environmentally friendly hemicellulose group hydrophobically modified thermo-sensitive gel is prepared, as pentachlorophenol, pentachlorodiphenyl, 3,4-
The polytype such as BaP HOCs adsorbent.It is not only to make up the vacancy that hemicellulose macromolecule is studied in heteroproteose cell, and
The comprehensive utilization ratio of maize straw resource is improved, positive impetus is played for the high value added utilization of the corn stalk stalks of rice, wheat, etc..
The content of the invention
For hemicellulose group thermo-sensitive gel developing also without enough bases as hydrophobic Adsorption of Organic agent
With the support of technology, therefore, effective reuse, the industry of environmentally friendly attractive gel also non-scale preferable with disposal ability
Using and exploitation.Therefore, the invention provides a kind of preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group, the party
Method is raw material using aboundresources but the still shallow corn stalk stalks of rice, wheat, etc. of Exploitation Depth, its hemicellulose of high efficiency extraction, then with hydrophobic list
Body, temperature sensitive monomer and crosslinking agent carry out graft copolymerization/cross-linking reaction, and hemicellulose group hydrophobically modified thermo-sensitive gel product is made；
The application field of hemicellulose is further expanded, lifts corn stalk stalks of rice, wheat, etc. added value.
Realize that the process technology scheme that the object of the invention is taken is as follows：
（1）Maize straw is removed the peel after air-drying, and straw stalks of rice, wheat, etc. partial mill and screening, obtains acceptable material；
（2）Qualified straw stalks of rice, wheat, etc. raw material carries out alkali and assists hot-water extraction hemicellulose separating treatment under given conditions, after processing
Material filter membrane separates, filtrate alcohol precipitation, centrifugation and washing, until cleaning solution is neutrality, sediment freeze-drying, corn is made
Straw stalks of rice, wheat, etc. hemicellulose, it is standby；
（3）Graft copolymerization is carried out to corn stalk stalks of rice, wheat, etc. hemicellulose using aqueous solution micellar copolymerization method, i.e., from persulfuric acid
Ammonium is accelerator as initiator, N, N, N, N ,-tetramethylethylenediamine, and N, N ,-methylene-bisacrylamide is crosslinking agent, and N- is different
Propylacrylamide is temperature sensitive monomer, and phenyl methacrylate is hydrophobic monomer, and ten disulfobenzene sodium sulfonates are surfactant,
Graft copolymerization/crosslinking inborn nature is carried out, copolymer products are washed, are freeze-dried respectively with absolute ethyl alcohol and water, obtain corn
The hydrophobic thermo-sensitive gel of straw stalks of rice, wheat, etc. hemicellulose group.
The preparation method of the above-mentioned hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group, concrete operations are as follows：
（1）The melting process of the corn stalk stalks of rice, wheat, etc.：Maize straw is after air-drying processing, wherein air-drying the moisture of raw material according to difference
Season air humidity is different and different from different places, and general moisture control is in the range of 5~30%, after air dry matter peeling,
Straw stalks of rice, wheat, etc. part, mechanical crushing grinding are obtained, and is screened by the screen cloth of 60~300 mesh, obtains acceptable material；
（2）Qualified straw stalks of rice, wheat, etc. raw material hemicellulose separation process：It is equal that air-dried straw stalks of rice, wheat, etc. raw material and potassium hydroxide, water are sufficiently mixed stirring
After even, cooker is transferred to completely（Sealed pressure vessel tank）In, sealing, it is put into rotation electric heater unit, in set point of temperature
It is with progress hemicellulose extraction process, treatment conditions under conditions of the time：Potassium hydroxide dosage is over dry corn stalk stalks of rice, wheat, etc. quality
1.0~10.0%, system reclaimed water and 5 ~ 15g of over dry corn stalk stalks of rice, wheat, etc. mass ratio:1g, 0.5~3.0h of reaction time, processing temperature
120~200 DEG C of degree；Material after being disposed is cooled to room temperature, and take off from oxygen be transferred to completely in tank aperture for 0.20~
Carry out separation of solid and liquid in 1.00nm filter membranes, liquid portion pours into absolute ethyl alcohol until white emulsion state occurs in transparency liquid, says
Bright precipitating finishes, and is washed with absolute ethyl alcohol and 10~20min is centrifuged under 7000~15000rpm, be neutrality to cleaning solution, cold
It is lyophilized dry until material is completely dried, produce corn stalk stalks of rice, wheat, etc. hemicellulose；
（3）The preparation process of the hydrophobic thermo-sensitive gel of hemicellulose group：By corn stalk stalks of rice, wheat, etc. hemicellulose, NIPA and
N, N- methylene-bisacrylamide dissolve in water, then inject phenyl methacrylate and ten disulfobenzene sodium sulfonates, logical
5 ~ 30min is stirred vigorously under the conditions of nitrogen, adds ammonium persulfate/N, N, N, N- tetramethylethylenediamines, initiation grafting copolyreaction；Its
In, NIPA is 1 with corn stalk stalks of rice, wheat, etc. hemicellulose mass ratio:1~10:1, phenyl methacrylate and corn stalk
Stalks of rice, wheat, etc. hemicellulose mass ratio is 3:1~15:1, ammonium persulfate is 0.005 with corn stalk stalks of rice, wheat, etc. hemicellulose mass ratio:1~0.025:
1；N,N methylene bis acrylamide quality is 0.005 with the ratio between temperature sensitive monomer and hydrophobic monomer quality summation:1~0.02:1,
N, N, N, N- tetramethylethylenediamine are 2 with ammonium persulfate mass ratio:1~1:2, reaction temperature is 40~70 DEG C, and the reaction time is
15.0~48.0h, the ratio between corn stalk stalks of rice, wheat, etc. hemicellulose quality and reaction liquid cumulative volume are controlled in 1g:50mL~1g:150mL's
In the range of, mass concentration of the ten disulfobenzene sodium sulfonates in reaction system is 3 ~ 8%；After completion of the reaction, gel be cut into 1.00~
2.00cm × 1.00~2.00cm × 0.10~1.00cm fritter, 12 are washed repeatedly to fritter synthetic with absolute ethyl alcohol
After ~ 72h, continue to carry out washing 2 ~ 8 days with water, be freeze-dried, produce the hydrophobic thermo-sensitive gel based on corn stalk stalks of rice, wheat, etc. hemicellulose.
The present invention is another object is that the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group made from the above method is applied
In adsorption treatment organic pollution.
The beneficial effects of the invention are as follows：It is short using high temperature using the agricultural wastes corn stalk stalks of rice, wheat, etc. as the source of hemicellulose
When under the conditions of alkali assist the isolated hemicellulose of hot-water extraction technology, by aqueous solution micellar copolymerization method, by temperature sensitive list
Phenyl methacrylate graft copolymerization is in hemicellulose macromolecular chain for body --- NIPA and hydrophobic monomer ---
On, and and N, N- methylene-bisacrylamide carry out cross-linking reaction, obtain adsorb HOCs corn stalk stalks of rice, wheat, etc. hemicellulose group it is hydrophobic
Thermo-sensitive gel.Hemicellulose has the general character of synthesis high score subclass sorbing material for " intelligence " attractive gel of matrix, can change
It can be played in terms of the processing of organic pollution waste liquid caused by multiple industries such as work, weaving, printing and dyeing, pharmacy, printing good
Application prospect.Meanwhile the attractive gel is also equipped with efficient absorption and desorption performance, reuse number are high, environment-friendly etc. excellent
Gesture, is a kind of new, green functional material of mainstream development now, and this attractive gel is embodied as maize straw high added value
One feasible scheme of offer is provided.
Embodiment
The present invention is described in further detail with reference to embodiment, but the scope of the present invention is not limited in described
Hold, the method used in the present embodiment is conventional method unless otherwise specified, and the reagent used is normal unless otherwise specified
Advise reagent.
Embodiment 1：It is as follows based on the preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose, concrete operations：
（1）The stock of the corn stalk stalks of rice, wheat, etc.
Maize straw is by air-drying processing, wherein the water content for air-drying raw material is 5%, after artificial peeling, the straw stalks of rice, wheat, etc. carries out mechanical grinding
Mill processing, it is then acceptable material after 60 mesh but the only screening of 100 eye mesh screens；
（2）The separation of corn stalk stalks of rice, wheat, etc. raw material hemicellulose
Hemicellulose extraction condition be：Potassium hydroxide dosage is the 1.0% of over dry material quality, system reclaimed water and over dry raw material
Mass ratio 5g:1g, reaction time 0.5h, 120 DEG C for the treatment of temperature.
Concrete operation step is：By 10.0g over dry straw stalks of rice, wheat, etc. raw materials（If it is 5% to air-dry raw material moisture, 10.5g is weighed
Air-dry the straw stalks of rice, wheat, etc.）, 0.1g potassium hydroxide（10×1.0%=0.1g）With 50mL water（10×5=50mL）It is sufficiently mixed uniformly, completely
It is transferred in cooker, seals, is put into rotation electric heater unit, starts to react after being warming up to 120 DEG C, reacted after 0.5h
Terminate, after material is cooled to room temperature, is taken off from oxygen and be transferred to aperture in tank completely to carry out separation of solid and liquid, liquid in 0.20nm filter membranes
Part pour into absolute ethyl alcohol until transparency liquid there is white emulsion state, washed with absolute ethyl alcohol and centrifuged under 7000rpm
10min, it is neutrality to clean to cleaning solution, freeze-drying, produces corn stalk stalks of rice, wheat, etc. hemicellulose.
（3）The preparation of the hydrophobic thermo-sensitive gel of hemicellulose group
Gel preparation condition：NIPA is 1 with hemicellulose mass ratio:1, phenyl methacrylate and hemicellulose
Plain mass ratio is 3:1, ammonium persulfate is 0.005 with hemicellulose mass ratio:1；N,N methylene bis acrylamide quality and temperature
The ratio between quick and hydrophobic two kinds of monomer mass summations are 0.005:1, N, N, N, N- tetramethylethylenediamine is with ammonium persulfate mass ratio
2:1, reaction temperature is 40 DEG C, reaction time 15.0h, and the ratio between hemicellulose quality and reaction liquid cumulative volume are controlled in 1g:
In the range of 50mL, mass concentration of the ten disulfobenzene sodium sulfonates in reaction system is 3%.
Gel preparation course：Equipped with reflux condensing tube, mechanical agitator three mouthfuls of reaction bulbs in add 5g hemicelluloses,
5g NIPAs（5×1=5g）With 0.1g N,N methylene bis acrylamides（0.005×（5+15）=0.1g）,
Add a certain amount of deionized water and fully dissolve reactant, then inject 15g phenyl methacrylates（5×3=15g）And 7.5g
Ten disulfobenzene sodium sulfonates（250×3%=7.5g）, reaction bulb is stirred vigorously in 40 DEG C of water bath with thermostatic control under nitrogen protection
0.025g ammonium persulfates are added after 5min（0.005×5=0.025g）With 0.05g N, N, N, N- tetramethylethylenediamines（0.025×
2=0.05g）, while deionized water is added, it is 250mL to make reaction solution cumulative volume（50×5=250mL）, react 15h；Graft copolymerization
After reaction, network body gel is cut into 1.00cm × 1.00cm × 0.10cm fritter, and after washing 12h repeatedly with absolute ethyl alcohol,
Continue to be washed with water 2 days, be freeze-dried, produce the hydrophobic thermo-sensitive gel of hemicellulose group.
（4）The character of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group
HOCs determining adsorption methods：Measure takes 2g or so desiccant gel to be immersed in the pentachloro- that 500mL concentration is 25mg/L respectively
In phenol, pentachlorodiphenyl, 3,4- BaP solution, shaking table rocks 24h under the conditions of 25 DEG C, after adsorption equilibrium, takes out gel, profit
With the content of remaining organic pollution in each solution of high performance liquid chromatography detection.
The hydrophobic thermo-sensitive gel of hemicellulose group as obtained by above-mentioned reaction has comparatively ideal HOCs adsorption capacities, to five
Chlorophenol, pentachlorodiphenyl, the removal efficiency of 3,4- BaPs respectively reach 82%, 79% and 76%, and physical behavior is white blocks
Shape.
Gel renovation process：Absorption HOCs gel is put into 50 DEG C of 300mL deionized water, after 24h, freezing
Dry, namely regenerated gel；Rejuvenation gel continues adsorption experiment in above-mentioned hydrophobic Adsorption of Organic method.
As a result can obtain：Reusable 5 times of the gel as obtained by above-mentioned reaction, to pentachlorophenol, pentachlorodiphenyl, 3,4- benzene
And the removal efficiency of pyrene is without being decreased obviously.
Embodiment 2：It is as follows based on the preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose, concrete operations：
（1）The stock of the corn stalk stalks of rice, wheat, etc.
Maize straw is by air-drying processing, wherein the water content for air-drying raw material is 20%, after artificial peeling, the straw stalks of rice, wheat, etc. carries out mechanical grinding
Mill processing, it is then acceptable material after 100 mesh but the only screening of 200 eye mesh screens；
（2）The separation of corn stalk stalks of rice, wheat, etc. raw material hemicellulose
Hemicellulose extraction condition be：Potassium hydroxide dosage is the 8.0% of over dry material quality, and water and over dry are former in system
Expect mass ratio 10g:1g, reaction time 2.0h, 170 DEG C for the treatment of temperature.
Concrete operation step is：By 10.0g over dry straw stalks of rice, wheat, etc. raw materials（If it is 20% to air-dry raw material moisture, 12.5g is weighed
Air-dry the straw stalks of rice, wheat, etc.）, 0.8g potassium hydroxide（10×8.0%=0.8g）With 100mL water（10×10=100mL）It is sufficiently mixed uniformly, it is complete
Total transfer is into cooker, sealing, is put into rotation electric heater unit, starts to react after being warming up to 170 DEG C, anti-after 2.0h
It should terminate, after material is cooled to room temperature, be taken off from oxygen and be transferred to aperture in tank completely to carry out separation of solid and liquid, liquid in 0.45nm filter membranes
Body portion pour into absolute ethyl alcohol until transparency liquid there is white emulsion state, washed with absolute ethyl alcohol and under 10000rpm from
Heart 15min, it is neutrality to clean to cleaning solution, freeze-drying, produces corn stalk stalks of rice, wheat, etc. hemicellulose.
（3）The preparation of the hydrophobic thermo-sensitive gel of hemicellulose group
Gel preparation condition：NIPA is 5 with hemicellulose mass ratio:1, phenyl methacrylate and hemicellulose
Plain mass ratio is 12:1, ammonium persulfate is 0.015 with hemicellulose mass ratio:1；N,N methylene bis acrylamide dosage and temperature
The ratio between quick and hydrophobic two kinds of monomer mass summations are 0.010:1, N, N, N, N- tetramethylethylenediamine is with ammonium persulfate mass ratio
1:1, reaction temperature is 55 DEG C, reaction time 24.0h, and the ratio between hemicellulose quality and reaction liquid cumulative volume are controlled in 1g:
In the range of 100mL, mass concentration of the ten disulfobenzene sodium sulfonates in reaction system is 5%.
Gel preparation course：Equipped with reflux condensing tube, mechanical agitator three mouthfuls of reaction bulbs in add 5g hemicelluloses,
25g NIPAs（5×5=25g）With 0.85g N,N methylene bis acrylamides（0.010×（25+60）=
0.85g）, add a certain amount of deionized water and fully dissolve reactant, then inject 60g phenyl methacrylates（5×12=
60g）With the disulfobenzene sodium sulfonates of 25g ten（500×5%=25g）, under nitrogen protection by reaction bulb in 55 DEG C of water bath with thermostatic control
0.025g ammonium persulfates are added after acutely stirring 20min（0.015×5=0.075g）With 0.075g N, N, N, N- tetramethylethylenediamines
（0.075×1=0.075g）, while deionized water is added, it is 250mL to make reaction solution cumulative volume（100×5=500mL）, reaction
24h；After graft copolymerization, network body gel is cut into 1.50cm × 1.50cm × 0.50cm fritter, and anti-with absolute ethyl alcohol
After 24h is washed in after backwashing, continue to be washed with water 5 days, be freeze-dried, produce the hydrophobic thermo-sensitive gel of hemicellulose group.
（4）The character of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group
HOCs determining adsorption methods：Measure takes 2g or so desiccant gel to be immersed in the pentachloro- that 500mL concentration is 25mg/L respectively
In phenol, pentachlorodiphenyl, 3,4- BaP solution, shaking table rocks 24h under the conditions of 25 DEG C, after adsorption equilibrium, takes out gel, profit
With the content of remaining organic pollution in each solution of high performance liquid chromatography detection.
The hydrophobic thermo-sensitive gel of hemicellulose group as obtained by above-mentioned reaction has comparatively ideal HOCs adsorption capacities, to five
Chlorophenol, pentachlorodiphenyl, the removal efficiency of 3,4- BaPs respectively reach 95%, 90% and 88%, and physical behavior is white blocks
Shape.
Gel renovation process：Absorption HOCs gel is put into 50 DEG C of 300mL deionized water, after 24h, freezing
Dry, namely regenerated gel；Rejuvenation gel continues adsorption experiment in above-mentioned hydrophobic Adsorption of Organic method.
As a result can obtain：Reusable 9 times of the gel as obtained by above-mentioned reaction, to pentachlorophenol, pentachlorodiphenyl, 3,4- benzene
And the removal efficiency of pyrene is without being decreased obviously.
Embodiment 3：It is as follows based on the preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose, concrete operations：
（1）The stock of the corn stalk stalks of rice, wheat, etc.
Maize straw is by air-drying processing, wherein the water content for air-drying raw material is 30%, after artificial peeling, the straw stalks of rice, wheat, etc. carries out mechanical grinding
Mill processing, it is then acceptable material after 200 mesh but the only screening of 300 eye mesh screens；
（2）The separation of corn stalk stalks of rice, wheat, etc. raw material hemicellulose
Hemicellulose extraction condition be：Potassium hydroxide dosage is the 10.0% of over dry material quality, water and over dry in system
The ratio between material quality 15g:1g, reaction time 3.0h, 200 DEG C for the treatment of temperature.
Concrete operation step is：By 10.0g over dry straw stalks of rice, wheat, etc. raw materials（If it is 30% to air-dry raw material moisture, 14.3g is weighed
Air-dry the straw stalks of rice, wheat, etc.）, 1.0g potassium hydroxide（10×10.0%=1.0g）With 150mL water（15×10=150mL）It is sufficiently mixed uniformly,
It is transferred in cooker, seals completely, is put into rotation electric heater unit, starts to react after being warming up to 200 DEG C, after 3.0h
Reaction terminates, and after material is cooled to room temperature, is taken off from oxygen and is transferred to aperture in tank completely to carry out separation of solid and liquid in 1.00nm filter membranes,
Liquid portion pour into absolute ethyl alcohol until transparency liquid there is white emulsion state, washed with absolute ethyl alcohol and under 15000rpm
20min is centrifuged, it is neutrality to clean to cleaning solution, freeze-drying, produces hemicellulose.
（3）The preparation of the hydrophobic thermo-sensitive gel of hemicellulose group
Gel preparation condition：NIPA dosage is 10 with hemicellulose mass ratio:1, phenyl methacrylate is used
Amount is 15 with hemicellulose mass ratio:1, ammonium persulfate dosage is 0.025 with hemicellulose mass ratio:1；N,N,- di-2-ethylhexylphosphine oxide
The ratio between acrylamide dosage and temperature sensitive and hydrophobic two kinds of monomer mass summations are 0.020:1, N, N, N, N- tetramethylethylenediamine with
Ammonium persulfate mass ratio is 1:2, reaction temperature is 70 DEG C, reaction time 48.0h, and hemicellulose quality and reaction liquid are total
The ratio between volume is controlled in 1g:In the range of 150mL, mass concentration of the ten disulfobenzene sodium sulfonates in reaction system is 8%.
Gel preparation course：Equipped with reflux condensing tube, mechanical agitator three mouthfuls of reaction bulbs in add 5g hemicelluloses,
50g NIPAs（10×5=50g）With 2.5g N,N methylene bis acrylamides（0.020×（50+75）=
2.5g）, add a certain amount of deionized water and fully dissolve reactant, then inject 75g phenyl methacrylates（5×15=75g）
With the disulfobenzene sodium sulfonates of 60g ten（750×8%=60g）, under nitrogen protection by reaction bulb in 70 DEG C of water bath with thermostatic control acutely
0.125g ammonium persulfates are added after stirring 30min（0.025×5=0.125g）With 0.063g N, N, N, N- tetramethylethylenediamines
（0.125×1/2=0.063g）, while deionized water is added, it is 750mL to make reaction solution cumulative volume（150×5=750mL）, reaction
48h；After graft copolymerization, network body gel is cut into 2.00cm × 2.00cm × 1.00cm fritter, and anti-with absolute ethyl alcohol
After 72h is washed in after backwashing, continue to be washed with water 8 days, be freeze-dried, produce the hydrophobic thermo-sensitive gel of hemicellulose group.
（4）The character of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group
HOCs determining adsorption methods：Measure takes 2g or so desiccant gel to be immersed in the pentachloro- that 500mL concentration is 25mg/L respectively
In phenol, pentachlorodiphenyl, 3,4- BaP solution, shaking table rocks 24h under the conditions of 25 DEG C, after adsorption equilibrium, takes out gel, profit
With the content of remaining organic pollution in each solution of high performance liquid chromatography detection.
The hydrophobic thermo-sensitive gel of hemicellulose group as obtained by above-mentioned reaction has comparatively ideal HOCs adsorption capacities, to five
Chlorophenol, pentachlorodiphenyl, the removal efficiency of 3,4- BaPs respectively reach 91%, 94% and 90%, and physical behavior is white blocks
Shape.
Gel renovation process：Absorption HOCs gel is put into 50 DEG C of 300mL deionized water, after 24h, freezing
Dry, namely regenerated gel；Rejuvenation gel continues adsorption experiment in above-mentioned hydrophobic Adsorption of Organic method.
As a result can obtain：Reusable 7 times of the gel as obtained by above-mentioned reaction, to pentachlorophenol, pentachlorodiphenyl, 3,4- benzene
And the removal efficiency of pyrene is without being decreased obviously.
Claims (3)
1. a kind of preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group, it is characterised in that carry out as follows：
1. maize straw air-dries dry after removed the peel, ground and screening process, qualified straw stalks of rice, wheat, etc. raw material assists hot water to take out using alkali
Extracting method carries out hemicellulose separating treatment, the material filter membrane separation after processing, filtrate alcohol precipitation, centrifugation and washing, until
Cleaning solution is neutrality, cleans sediment freeze-drying, corn stalk stalks of rice, wheat, etc. hemicellulose is made；
2. graft copolymerization is carried out to corn stalk stalks of rice, wheat, etc. hemicellulose using aqueous solution micellar copolymerization method, it is fine with the corn stalk stalks of rice, wheat, etc. half
It is response matrix to tie up element, and from ammonium persulfate as initiator, N, N, N, N- tetramethylethylenediamines are accelerator, N, N- methylene
Bisacrylamide is crosslinking agent, and NIPA is temperature sensitive monomer, and phenyl methacrylate is hydrophobic monomer, 12 sulphurs
Base benzene sulfonic acid sodium salt is surfactant, carries out graft copolymerization/crosslinking inborn nature, and copolymer products are carried out respectively with absolute ethyl alcohol and water
Washing, freeze-drying, obtain the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group.
2. the preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group according to claim 1, it is characterised in that
Concrete operations are as follows：
1. the maize straw after air-dried processing is removed the peel, ground, and by the sieved through sieve of 60~300 mesh, obtain qualified original
Material；
2. air-dried straw stalks of rice, wheat, etc. raw material and potassium hydroxide, water are sufficiently mixed after stirring, it is transferred in cooker, seals completely,
It is put into rotation electric heater unit and carries out hemicellulose extraction process, wherein, potassium hydroxide dosage is over dry corn stalk stalks of rice, wheat, etc. quality
1.0~10.0%, the mass ratio of water and the over dry corn stalk stalks of rice, wheat, etc. is 5 ~ 15:1,0.5~3.0h of reaction time, treatment temperature 120
~200 DEG C；Material after being disposed is cooled to room temperature, and is transferred to aperture completely to be consolidated in 0.20~1.00nm filter membranes
Liquid separates, and liquid portion pours into absolute ethyl alcohol until white emulsion state is presented in transparency liquid, and precipitating is finished, washed with absolute ethyl alcohol
Wash and centrifuged under 7000~15000rpm, be neutrality to cleaning solution, freeze-drying is completely dried up to material, produces corn stalk
Stalks of rice, wheat, etc. hemicellulose；
3. corn stalk stalks of rice, wheat, etc. hemicellulose, NIPA and N, N- methylene-bisacrylamide are dissolved in water, after
And phenyl methacrylate and ten disulfobenzene sodium sulfonates are injected, 5 ~ 30min is stirred vigorously under the conditions of logical nitrogen, adds persulfuric acid
Ammonium and N, N, N, N- tetramethylethylenediamine, initiation grafting copolyreaction, wherein, NIPA and the corn stalk stalks of rice, wheat, etc. half are fine
The mass ratio of dimension element is 1:1~10:1, phenyl methacrylate is 3 with corn stalk stalks of rice, wheat, etc. hemicellulose mass ratio:1~15:1, mistake
Ammonium sulfate is 0.005 with corn stalk stalks of rice, wheat, etc. hemicellulose mass ratio:1~0.025:1；N,N methylene bis acrylamide quality:Temperature
The ratio between quick monomer and hydrophobic monomer quality summation is 0.005:1~0.02:1, N, N, N, N- tetramethylethylenediamine and ammonium persulfate
Mass ratio is 2:1~1:2, reaction temperature is 40~70 DEG C, and the reaction time is 15.0~48.0h, corn stalk stalks of rice, wheat, etc. hemicellulose quality
With the control of the ratio between reaction liquid cumulative volume in 1g:50mL~1g:In 150mL, ten disulfobenzene sodium sulfonates are in reaction system
Mass concentration is 3 ~ 8%；After completion of the reaction, gel is cut into small pieces, fritter synthetic is carried out with absolute ethyl alcohol repeatedly washing 12 ~
After 72h, continue to carry out washing 2 ~ 8 days with water, be freeze-dried, obtain the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group.
3. corn stalk made from the preparation method of the hydrophobic thermo-sensitive gel of corn stalk stalks of rice, wheat, etc. hemicellulose group described in claim 1 or 2
Application of the hydrophobic thermo-sensitive gel of stalks of rice, wheat, etc. hemicellulose group in adsorption treatment organic pollution.
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| CN110065988A (en) * | 2019-04-23 | 2019-07-30 | 中国石油大学(华东) | A method of going heavy metal ion in water removal |
| CN110170303A (en) * | 2019-06-10 | 2019-08-27 | 陕西科技大学 | A kind of heavy-metal adsorption material and its preparation method and application |
| CN110372049A (en) * | 2019-07-12 | 2019-10-25 | 中国农业科学院农业环境与可持续发展研究所 | A kind of preparation method and application of high-performance cadmium fixative |
| CN110372049B (en) * | 2019-07-12 | 2021-09-28 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method and application of high-performance cadmium fixing agent |
| CN113318784A (en) * | 2021-05-27 | 2021-08-31 | 昆明理工大学 | Preparation method and application of corn straw loaded nano osmium composite filter column |
| CN113318784B (en) * | 2021-05-27 | 2022-07-05 | 昆明理工大学 | Preparation method and application of corn straw loaded nano osmium composite filter column |
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