CN110078974A - Sesbania gum/cellulose composite water conservation hydrogel preparation method - Google Patents
Sesbania gum/cellulose composite water conservation hydrogel preparation method Download PDFInfo
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- CN110078974A CN110078974A CN201910219647.6A CN201910219647A CN110078974A CN 110078974 A CN110078974 A CN 110078974A CN 201910219647 A CN201910219647 A CN 201910219647A CN 110078974 A CN110078974 A CN 110078974A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 95
- 239000001913 cellulose Substances 0.000 title claims abstract description 94
- 241000219782 Sesbania Species 0.000 title claims abstract description 81
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910001868 water Inorganic materials 0.000 title claims abstract description 47
- 239000000017 hydrogel Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 52
- 235000009566 rice Nutrition 0.000 claims abstract description 52
- 241000209140 Triticum Species 0.000 claims abstract description 50
- 235000021307 Triticum Nutrition 0.000 claims abstract description 50
- 240000008042 Zea mays Species 0.000 claims abstract description 50
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 50
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 50
- 235000005822 corn Nutrition 0.000 claims abstract description 50
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000010907 stover Substances 0.000 claims abstract description 15
- 239000010902 straw Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract 3
- 239000000243 solution Substances 0.000 claims description 78
- 241000209094 Oryza Species 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000004090 dissolution Methods 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000000499 gel Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000007872 degassing Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 9
- 239000004971 Cross linker Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- 239000003599 detergent Substances 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- GPFIZJURHXINSQ-UHFFFAOYSA-N acetic acid;nitric acid Chemical compound CC(O)=O.O[N+]([O-])=O GPFIZJURHXINSQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000004132 cross linking Methods 0.000 abstract description 7
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002689 soil Substances 0.000 abstract description 5
- 241000196324 Embryophyta Species 0.000 abstract description 3
- 239000000284 extract Substances 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract description 2
- 230000012010 growth Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 240000007594 Oryza sativa Species 0.000 abstract 3
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 235000010980 cellulose Nutrition 0.000 description 70
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 238000007654 immersion Methods 0.000 description 9
- 230000008961 swelling Effects 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 239000004809 Teflon Substances 0.000 description 4
- 229920006362 Teflon® Polymers 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 210000000630 fibrocyte Anatomy 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 229920005615 natural polymer Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- -1 N, N'- methylene Chemical group 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 150000008131 glucosides Chemical class 0.000 description 2
- 238000005213 imbibition Methods 0.000 description 2
- 239000010977 jade Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 2
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 1
- 240000003133 Elaeis guineensis Species 0.000 description 1
- 235000001950 Elaeis guineensis Nutrition 0.000 description 1
- 229920000926 Galactomannan Polymers 0.000 description 1
- 229920002907 Guar gum Polymers 0.000 description 1
- 208000029422 Hypernatremia Diseases 0.000 description 1
- 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 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 229920001477 hydrophilic polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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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
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of sesbania gum/cellulose composite water conservation hydrogel preparation methods, after corn stover is air-dried disleaf peeling by this method, the straw stalks of rice, wheat, etc. raw material sheared to it, be ground up, sieved qualified then handles to obtain corn stalk stalks of rice, wheat, etc. cellulose using acetic/nitric acid mixture；By cellulose and sesbania gum respectively in the NaOH- urea-H of pre-cooling2It is dissolved in O mixed solution, is mixed later, epoxychloropropane is added and is stirred, is centrifuged and heating makes its crosslinking；End of reaction, product through impurity elimination, clean after sesbania gum/cellulose composite water conservation hydrogel；This method is raw material using agriculture waste biomass corn stover resourceful but that exploitation degree is still shallow, it extracts straw stalks of rice, wheat, etc. cellulose and mixes crosslinking with sesbania gum to prepare hydrogel with high-moisture-retention and degradable, as water-keeping material effective in agriculture and forestry, facilitate the reasonable efficient growth using with plant of soil moisture.
Description
Technical field
The present invention relates to a kind of techniques of gel rubber material by the compound preparation of sesbania gum and cellulose with high-water performance
Method belongs to natural macromolecular material technical field.
Background technique
With the fast development of China's economic, to water-saving irrigation, more stringent requirements are proposed for agricultural production, only efficiently sharp
It just will not underproduction due to water shortage with water resource.But water shortage is one of the agricultural problem of most serious in the world.Substitution tradition is poured
The application study of method will become more important.In recent years, the high absorbency materials such as hydrophilic polymer are because it is with retain water and nutrients
Characteristic, plant growth can be promoted and received significant attention.Hydrogel is that have hydrophily and the three-dimensional network of high-expansion parent
Aqueous polymer.Due to its porous structure and superabsorbent, they can be absorbed and retain a large amount of water.At past 40 years
In, hydrogel is widely used in agriculture and forestry, it is intended to the utilization efficiency of water is improved, because the hydrogel of swelling can be used as a storage
Hydrophone, it can adjust water release rate according to the dry and wet degree of soil, and water conservancy is used in plant normal growth by specific aim, can be big
Improve to amplitude the utilization efficiency of water resource.It is and natural however, most of hydrogels are prepared by synthetic polymer in the market
Polymer phase ratio, their biocompatibility and biological degradability are not ideal.Realize biodegradable natural polymer
Can part so that the nondegradable synthetic macromolecule resin of replacing whole, realize renewable resource sustainability conversion and benefit
With one of the trend for having become development of modern scientific technology.
Sesbania gum is a kind of polysaccharide colloid by extracting in the endosperm of leguminous plant sesbania, is that China is distinctive
Natural polysaccharide, average molecular weight are 2.3 × 105~3.4×105, and most of is galactomannans and its primary structure
Side chain including β (1 → 4) glucosides key connection mannose and α (1 → 6) glucosides key connection galactolipin.Its physicochemical property and chemistry knot
Structure is similar to guar gum, it is worth noting that sesbania gum makes it have excellent guarantor because of its significant expansion rate and high viscosity
It is aqueous, in terms of the research and development that can be applied to water-retaining agent.However, sesbania gum also shows " Weak Gels " shape characteristic, so that plastic
Intensity is too low, and colloidal stability is on the weak side, and plastic speed and gelation time are also not satisfactory.To solve the above-mentioned problems, sesbania
Glue usually requires to combine the high molecular material of mechanical stable structure, is compounded to form the gel of tough and tensile dual network body, keeps its hydrophilic
Performance is put to good use.For example, experimental studies have found that, cellulose can enhance the bone of its porous structure in conjunction with sesbania gum by this
Frame.
As natural polymer the most abundant on the earth, cellulose is considered as inexhaustible raw material, and cellulose base is multiple
Condensation material the advantages that biodegradable and good biocompatibility and is received more and more attention because its is nontoxic.Nowadays, fiber
Plain based aquagel is studied and is applied in different field.For example, Wuhan University Chang Chunyu is with sodium carboxymethylcellulose (CMC)
It is raw material with cellulose, using epoxychloropropane as crosslinking agent, successfully preparing in sodium hydroxide/aqueous solution of urea system has
The novel super absorbent gel of stronger adsorption capacity and higher equilibrium swelling rate.K.M. Salleh will be dissolved in hydroxide
Oil palm fruit (EFB) cellulose in sodium/urea solvent is mixed with sodium carboxymethylcellulose, in the crosslinked action of epoxychloropropane
Under, green regenerating high-hydroscopicity hydrogel is prepared, has further inquired into influence of the crosslinker concentration to water imbibition, finds water
Gel water imbibition increases with the increase of crosslinker concentration.Zhang Mingyue etc. is studied in composite initiator (2,2- dimethoxy -2-
Phenyl acetophenone and ammonium persulfate) and crosslinking agent (N, N'- methylene diene bisacrylamide) under the action of, with ultraviolet radioactive method will
Acrylic acid and corn bran are copolymerized, and are prepared for a kind of quick property of good salt and water retention property of showing under high-temperature and high-pressure conditions
Composite aquogel.Although very extensive, the Compound Water with sesbania gum is applied in the research of cellulose base hydrogel
Gel yet there are no relevant report.
In recent decades, in the country of the timber such as China shortage, the agriculture wastes such as stalk, straw, reed biomass is always
It is important fibre resources.A kind of discarded money of the renewable cultural solid that corn stover is huge as stock number but utilization rate is low
Source, cellulose rich in, and the corn stover major part in China is abandoned in ground or on-site incineration, only small part is used for
The industry such as feed processing, alcoholic fermentation, allow in this way corn stover this living resources do not obtain it is effective and high additional
Value utilizes.By a large amount of the study found that the bast of corn stover is substantially made of fibrocyte, marrow core is then mostly by non-fiber
Cell (or referred to as heteroproteose cell) is constituted, and the two cell is all different on construction and character.Fibrocyte is in thin fusiform, main
The supporting role of plant is played, single fiber intensity is larger；Heteroproteose cell wall construction is loose, and specific surface area is big compared with fibrocyte,
Free hydroxyl can be exposed to the maximum extent by resulting in its cellulose, increased the accessibility of reaction, increased derivative reaction
Uniformity and operability promote cellulose modified degree.Based on the characteristic of above-mentioned heteroproteose cell, we are just by corn stover
Stalks of rice, wheat, etc. portion cellulose is modified by advanced treating, with stronger or more hydrophilic radical, improves its water absorbing properties, with
Sesbania gum, which is cross-linked with each other, prepares hydrogel, is allowed to play bigger effect, play actively for the high value added utilization of corn stover
Impetus.
Can have in conjunction with the super water-absorbent of sesbania gum with the modified cellulose for similarly having high-hydroscopicity energy to prepare
High-moisture-retention and degradable hydrogel yet there are no relevant report.
Summary of the invention
Facilitate the absorption of water based on sesbania gum, and cellulose is as the skeletal substance for enhancing porous structure；The present invention is
A kind of novel cellulose base high-hydroscopicity hydrogel offer feasible scheme is provided, and provides a kind of sesbania gum/cellulose
The preparation method of composite water conservation hydrogel, product made from this method can be used as effective water-absorbing resins in agricultural；And
And the corn stalk stalks of rice, wheat, etc. for selecting resourceful but Exploitation Depth still shallow is raw material, extracts the cellulose in its heteroproteose cell, prepares fiber
Element crosslinking sesbania gum, obtains the product of composite hydrogel, further expands the application field of corn stover, make this green of stalk
Recyclable materials obtain the utilization of high added value.
Sesbania gum of the present invention/cellulose composite water conservation hydrogel the preparation method is as follows:
(1) corn stover skin stalk splitter after air-drying disleaf, selection straw stalks of rice, wheat, etc. part are primary raw material, it is sheared, is ground,
Sieving processing, obtains qualified corn stalk stalks of rice, wheat, etc. cellulosic material；
(2) it is handled under given conditions using the acetic acid-nitric acid mixture corn stalk stalks of rice, wheat, etc. cellulosic material qualified to stock, it
Afterwards successively with deionized water and ethanol washing reaction product to neutrality, corn stalk stalks of rice, wheat, etc. cellulose is obtained after drying；
(3) dry corn stalk stalks of rice, wheat, etc. cellulose and sesbania gum are dissolved in the NaOH- urea-H of pre-cooling respectively2In O mixed solution,
Cellulose solution and sesbania sol solution is made；
(4) it after carrying out centrifugation degassing process respectively to cellulose solution and sesbania sol solution, is then mixed by a certain percentage
Uniformly, centrifugation degassing process is carried out again after epichlorohydrin crosslinker stirring a period of time being added in the mixture, and gained is mixed
It closes object to heat within specified temperatures, reaction terminates, and gel is washed with deionized to neutrality, it is multiple that sesbania gum/cellulose is made
Close water-retaining property hydrogel.
The concrete operations of the above method are as follows:
(1) melting process of corn stover: corn stover is after air-drying processing, wherein air-drying the moisture of raw material because different
Regional, different seasons and air humidity are different and generate range of the general moisture control of certain difference 3~30%
Interior, air dry matter carries out skin stalks of rice, wheat, etc. lift-off processing, chooses straw stalks of rice, wheat, etc. part, cuts into segment and ground, by the sieve of 40 ~ 400 mesh
It is corn stalk stalks of rice, wheat, etc. cellulosic material after screening；
(2) extraction process of cellulose: taking 30 ~ 50 g step (1) corn stalk stalks of rice, wheat, etc. cellulosic materials to be put in heat-resistant glass tube, with
The nitric acid solution of the acetic acid solution of addition mass concentration 70 ~ 90% and mass concentration 60 ~ 80% afterwards, acetic acid solution and nitric acid solution
Volume ratio is 8:1 ~ 12:1；Using the screw lid equipped with teflon gasket by the glass seal of tube, be placed in temperature be 100 ~
15 ~ 30min is reacted in 120 DEG C of oil bath, glass tube is taken out from oil bath and cooling, and deionized water and anhydrous is then successively used
The thorough washing reaction product of ethyl alcohol is to neutrality.The product washed is placed in in 45 ~ 65 DEG C of baking oven dry 15 ~ 20h, jade is made
Rice straw stalks of rice, wheat, etc. cellulose；
(3) dissolution process of cellulose: step (2) corn stalk stalks of rice, wheat, etc. cellulose dissolution is urinated in the NaOH- for being cooled to -15 ~ -10 DEG C in advance
Element-H2In O mixed solution, the amount ratio g:mL of corn stalk stalks of rice, wheat, etc. cellulose and mixed solution is 1:20 ~ 1:50, be stirred continuously until
Cellulose solution is made in dissolution；
(4) it sesbania gum dissolution process: weighs dry sesbania gum and is dissolved in the pre- NaOH- urine for being cooled to -15 ~ -10 DEG C at 20 ~ 35 DEG C
Element-H2To being completely dissolved in O mixed solution and with magnetic stirrer, the amount ratio g:mL of sesbania gum and mixed solution is 1:
Sesbania sol solution is made in 25 ~ 1:35；
NaOH- urea-the H2O mixed solution is NaOH, urea, H2O is mixed in the ratio that g:g:mL is 1:1.5:10 ~ 1:2:12
It closes and is made；
(5) sesbania sol solution prepares the process of composite hydrogel with cellulose solution mixing crosslinking: by sesbania sol solution and fiber
Plain solution is centrifuged 10 ~ 20 min of degassing under conditions of 5000 ~ 10000rmp, 3 ~ 10 DEG C respectively, by sesbania sol solution and fiber
Plain solution mixes (solid masses of sesbania gum and cellulose ratio g:g is 1:2 ~ 1:10 in solution) in proportion and obtains sesbania gum/fibre
Tie up plain complex solution；Then epichlorohydrin crosslinker is added in sesbania gum/cellulose composite solution, crosslinking agent with
Sesbania gum/cellulose composite solution volume ratio be 1:15 ~ 1:25, after mixing, again 5000 ~ 10000rmp, 3 ~
10 ~ 20min of centrifugation degassing will be coagulated after gained mixture is heated 1 ~ 3h at 50 ~ 70 DEG C with deionized water under conditions of 10 DEG C
Glue is washed to neutrality, and sesbania gum/cellulose composite water conservation hydrogel is made.
Profitable fruit of the invention: using the straw stalks of rice, wheat, etc. in agricultural wastes corn stover as cellulose origin, using nitric acid/
Acetic extracts its straw stalks of rice, wheat, etc. cellulose, so by will it is cellulose modified after with the sesbania gum of dissolution in epoxychloropropane as friendship
Full cross-linked under conditions of connection agent that the significant environment-friendly type water gel of Water-saving effect is prepared, the hydrogel is by natural polymer fibre
Dimension element and sesbania compose, and have biocompatibility more better than conventional hydrogels, and biodegradable, are mainstream developments now
Novel, the green environmentally friendly functional material of one kind, can be applied to the agricultures such as desert afforestation, soil improvement, water and soil conservation more
On woods water-loss reducer of soil；The corn stalk stalks of rice, wheat, etc. high value added utilization that is embodied as of this composite hydrogel provides a feasible scheme,
The functionalization exploitation for also abandoning stalk and polysaccharide polymer simultaneously for other agricultures provides certain basis early period.
Specific embodiment
Below with reference to embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1: this sesbania gum/cellulose composite water conservation hydrogel the preparation method is as follows:
(1) process of the stock of the corn stalk stalks of rice, wheat, etc.
Skin stalk splitter after treated stalk disleaf will be air-dried, selections straw stalks of rice, wheat, etc. part is primary raw material, wherein air-dried raw material contains
Water rate is 3%, is then sheared and be ground up, sieved processing, and choosing through 40 ~ 80 mesh sieve is that the qualified corn stalk stalks of rice, wheat, etc. is fine
Tie up plain raw material；
(2) extraction process of cellulose
It weighs 30g step (1) corn stalk stalks of rice, wheat, etc. cellulosic material to be put in heat-resistant glass tube, 40mL mass concentration, which is then added, is
70% acetic acid solution and the nitric acid solution of 5mL mass concentration 60%；Using the screw lid equipped with teflon gasket by glass
The seal of tube is placed in the oil bath that temperature is 100 DEG C and reacts 25min, and glass tube is taken out and cooled down from oil bath, is then successively used
The product washed is placed in 45 DEG C of baking oven dry by deionized water and the thorough washing reaction product of dehydrated alcohol to neutrality
Corn stalk stalks of rice, wheat, etc. cellulose is made in 20h；
(3) course of dissolution of cellulose
4g step (2) corn stalk stalks of rice, wheat, etc. cellulose is taken, is dissolved in the solution by the mixing of 8g NaOH, 12g urea and 80mL water,
And mixed solution is first pre-chilled under conditions of -15 DEG C；Then continuous stirring is until dissolution, is made cellulose solution；
(4) course of dissolution of sesbania gum
The sesbania gum for taking 3.2g dry is dissolved in step (3) identical 80mL pre-cooled mixed solution at 20 DEG C, and uses magnetic
Power blender stirs to being completely dissolved to arrive sesbania sol solution；
(5) sesbania gum prepares the process of composite hydrogel with cellulose solution mixing crosslinking
Sesbania sol solution is centrifuged 20min respectively with cellulose solution to take off under conditions of temperature is 3 DEG C, revolving speed is 5000rmp
Gas；Then it measures 50mL sesbania sol solution to mix with 80mL cellulose solution, then 8.7mL epichlorohydrin crosslinker is added
Into mixed solution, after mixing, 20min degassing is centrifuged at 5000rmp, 3 DEG C again；By gained mixture at 50 DEG C
3h is heated, with deionized water by gel detergent to neutrality, sesbania gum/cellulose composite water conservation hydrogel is made；
(6) sesbania gum/cellulose composite water conservation hydrogel swelling ratio that this example is prepared is measured
The hydrogel that this example is prepared is put in distilled water, NaCl solution and CaCl respectively2The immersion of solution one week calculates
Obtain swelling ratio data are as follows: distilled water immersion is 120g/g；The immersion of NaCl solution is 85g/g；CaCl2What solution impregnated
For 80 g/g.
Embodiment 2: this cyanines glue/cellulose composite water conservation hydrogel preparation method, concrete operations are as follows:
(1) process of the stock of the corn stalk stalks of rice, wheat, etc.
Skin stalk splitter after treated stalk disleaf will be air-dried, selections straw stalks of rice, wheat, etc. part is primary raw material, wherein air-dried raw material contains
Water rate is 15%, is then sheared and be ground up, sieved processing, and choosing through 100 ~ 200 mesh sieve is the qualified corn stalk stalks of rice, wheat, etc.
Cellulosic material；
(2) extraction process of cellulose
It weighs 40g step (1) corn stalk stalks of rice, wheat, etc. cellulosic material to be put in heat-resistant glass tube, 80mL mass concentration 80% is then added
Acetic acid solution and 8mL 70% nitric acid solution；Using the screw lid equipped with teflon gasket by the glass seal of tube, juxtaposition
20min is reacted in the oil bath that temperature is 110 DEG C, glass tube is taken out and cooled down from oil bath, deionized water is then successively used
With the thorough washing reaction product of dehydrated alcohol to neutrality, the product washed is placed in in 55 DEG C of baking oven dry 18h, jade is made
Rice straw stalks of rice, wheat, etc. cellulose；
(3) course of dissolution of cellulose
6g step (2) corn stalk stalks of rice, wheat, etc. cellulose is taken, is dissolved in molten by the mixing of 21.8g NaOH, 39.3g urea and 240mL water
In liquid, and mixed solution will be pre-chilled under conditions of -12 DEG C；Then continuous stirring is until dissolution, is made cellulose solution；
(4) course of dissolution of sesbania gum
It takes the dry sesbania gum of 8g to be dissolved at 25 DEG C with step (3) identical 240mL pre-cooled mixed solution, and is stirred with magnetic force
It mixes device to stir to being completely dissolved, sesbania sol solution is made；
(5) sesbania gum prepares the process of composite hydrogel with cellulose solution mixing crosslinking
The sesbania sol solution and cellulose solution of dissolution are centrifuged under conditions of temperature is 5 DEG C, revolving speed is 8000rmp respectively de-
Gas 15min；Then it measures 30mL sesbania sol solution to mix with 240mL cellulose solution, then hands over 13.5mL epoxychloropropane
Connection agent is added in mixed solution, after mixing, again with 8000rmp, 5 DEG C of centrifugations degassing 15min；By gained mixture
2h is heated at 60 DEG C, with deionized water by gel detergent to neutrality, sesbania gum/cellulose composite water conservation hydrogel is made；
(6) sesbania gum/cellulose composite hydrogel swelling ratio that this example is prepared is measured
The hydrogel that this example is prepared is put in distilled water, NaCl solution and CaCl respectively2The immersion of solution one week calculates
Obtain swelling ratio data are as follows: distilled water immersion is 550g/g；The immersion of NaCl solution is 465g/g；CaCl2What solution impregnated
For 390g/g.
Embodiment 3: this sesbania gum/cellulose composite water conservation hydrogel preparation method, concrete operations are as follows:
(1) process of the stock of the corn stalk stalks of rice, wheat, etc.
Skin stalk splitter after treated stalk disleaf will be air-dried, selections straw stalks of rice, wheat, etc. part is primary raw material, wherein air-dried raw material contains
Water rate is 30%, is then sheared and be ground up, sieved processing, and choosing through 200 ~ 400 mesh sieve is the qualified corn stalk stalks of rice, wheat, etc.
Cellulosic material；
(2) extraction process of cellulose
It weighs 50 g step (1) corn stalk stalks of rice, wheat, etc. cellulosic materials to be put in heat-resistant glass tube, 120 mL mass concentrations is then added
The nitric acid solution of 90% acetic acid solution and 10 mL mass concentrations 60%；It will be managed using the screw lid equipped with teflon gasket
Sealing is placed in the oil bath that temperature is 120 DEG C and reacts 15min, and glass tube is taken out and cooled down from oil bath, is then successively used
Deionized water and the thorough washing reaction product of dehydrated alcohol are to neutrality；The product washed is placed in 65 DEG C of baking oven dry
15 hours to get corn stalk stalks of rice, wheat, etc. cellulose；
(3) course of dissolution of cellulose
9 g step (2) corn stalk stalks of rice, wheat, etc. celluloses are taken, are dissolved in by the mixing of 37.5 g NaOH, 75 g urea and 450 mL water
In solution, and mixed solution will be pre-chilled under conditions of -10 DEG C；Then continuous stirring is until dissolution, it is molten to be made cellulose
Liquid；
(4) course of dissolution of sesbania gum
It takes the dry sesbania gum of 12.86 g to be dissolved at 35 DEG C with step (3) identical 450mL pre-cooled mixed solution, and uses
Sesbania sol solution is made to being completely dissolved in magnetic stirrer；
(5) sesbania gum prepares the process of composite hydrogel with cellulose solution mixing crosslinking
Sesbania sol solution and cellulose solution are centrifuged 10min under conditions of temperature is 10 DEG C, revolving speed is 10000 rmp respectively
Degassing；Then it measures 32 mL sesbania sol solutions to mix with 450 mL cellulose solutions, then by 19mL epichlorohydrin crosslinker
It is added in mixed solution, after mixing, again with 10000 rmp, 10 DEG C of 15 min of centrifugation degassings；Gained mixture is existed
1 h is heated at 70 DEG C, and with deionized water by gel detergent to neutrality, sesbania gum/cellulose composite water conservation hydrogel is made；
(6) sesbania gum/cellulose composite hydrogel swelling ratio that this example is prepared is measured
The hydrogel that this example is prepared is put in distilled water, NaCl solution and CaCl respectively2The immersion of solution one week calculates
Obtain swelling ratio data are as follows: distilled water immersion is 320 g/g；The immersion of NaCl solution is 220 g/g；CaCl2Solution impregnates
It is 180 g/g.
Claims (3)
1. a kind of sesbania gum/cellulose composite water conservation hydrogel preparation method, it is characterised in that carry out as follows:
(1) corn stover skin stalk splitter after air-drying disleaf, selection straw stalks of rice, wheat, etc. part are raw material, are sheared, are ground to it, mistake
Corn stalk stalks of rice, wheat, etc. cellulosic material is made in sieve；To corn stalk stalks of rice, wheat, etc. cellulosic material using acetic acid-nitric acid mixture handle, then according to
It is secondary to use deionized water and ethanol washing reaction product to neutrality, corn stalk stalks of rice, wheat, etc. cellulose is obtained after drying；
(2) dry corn stalk stalks of rice, wheat, etc. cellulose and sesbania gum are dissolved in the NaOH- urea-H of pre-cooling respectively2In O mixed solution,
Cellulose solution and sesbania sol solution is made；
(3) it after carrying out centrifugation degassing process respectively to cellulose solution and sesbania sol solution, is uniformly mixed, is added in the mixture
Epichlorohydrin crosslinker carries out centrifugation degassing after stirring and evenly mixing again, carries out heating reaction to gained mixture, and reaction terminates, and uses
Sesbania gum/cellulose composite water conservation hydrogel is made to neutrality in deionized water detergent gel.
2. sesbania gum according to claim 1/cellulose composite water conservation hydrogel preparation method, it is characterised in that tool
Steps are as follows for body:
(1) for corn stover after air-drying processing, moisture control carries out skin in the range of 3~30% after air dry matter disleaf
Stalks of rice, wheat, etc. lift-off processing chooses straw stalks of rice, wheat, etc. part, cuts into segment and ground, and crosses 40 ~ 400 meshes, is corn stalk stalks of rice, wheat, etc. fiber after screening
Plain raw material；
(2) 30 ~ 50g step (1) corn stalk stalks of rice, wheat, etc. cellulosic material is taken to be put in heat-resistant glass tube, subsequent addition mass concentration 70 ~
The volume ratio of 90% acetic acid solution and the nitric acid solution of mass concentration 60 ~ 80%, acetic acid solution and nitric acid solution is 8:1 ~ 12:1；
The glass seal of tube is placed on 15 ~ 30min of reaction in 100 ~ 120 DEG C of oil baths, glass tube is taken out and cooled down from oil bath, then
Successively use deionized water and dehydrated alcohol washing reaction product to neutrality；The product washed is placed at 45 ~ 65 DEG C dry 15 ~
Corn stalk stalks of rice, wheat, etc. cellulose is made in 20 h；
(3) step (2) corn stalk stalks of rice, wheat, etc. cellulose dissolution is being cooled to -15 ~ -10 DEG C of NaOH- urea-H in advance2In O mixed solution,
The amount ratio g:mL of corn stalk stalks of rice, wheat, etc. cellulose and mixed solution is 1:20 ~ 1:50, is stirred continuously until dissolution, it is molten to be made cellulose
Liquid；
(4) by dry sesbania gum, magnetic agitation dissolves NaOH- urea-H at 20 ~ 35 DEG C2In O mixed solution, sesbania gum and mixed
The amount ratio g:mL for closing solution is 1:25 ~ 1:35, and sesbania sol solution is made；
(5) by sesbania sol solution and cellulose solution respectively under conditions of 5000 ~ 10000rmp, 3 ~ 10 DEG C centrifugation degassing 10 ~
20 min；Then the ratio for being 1:2 ~ 1:10 in the solid masses of sesbania gum in solution and cellulose ratio, by sesbania sol solution and
Cellulose solution is uniformly mixed, and sesbania gum/cellulose composite solution is made；Epichlorohydrin crosslinker is added to sesbania
In glue/cellulose composite solution, crosslinking agent and sesbania gum/cellulose composite solution volume ratio are 1:15 ~ 1:25, mixing
After uniformly, 10 ~ 20min of degassing is centrifuged under conditions of 5000 ~ 10000rmp, 3 ~ 10 DEG C again, by gained mixture 50 ~ 70
After heating 1 ~ 3h at DEG C, with deionized water by gel detergent to neutrality, sesbania gum/cellulose composite water conservation hydrogel is made.
3. sesbania gum according to claim 2/cellulose composite water conservation hydrogel preparation method, it is characterised in that:
NaOH- urea-H2O mixed solution is NaOH, urea, H2O is mixed to prepare in the ratio that g:g:mL is 1:1.5:10 ~ 1:2:12.
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