CN101524634A - Maize straw core absorbing material and preparing method thereof - Google Patents
Maize straw core absorbing material and preparing method thereof Download PDFInfo
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- CN101524634A CN101524634A CN200810242760A CN200810242760A CN101524634A CN 101524634 A CN101524634 A CN 101524634A CN 200810242760 A CN200810242760 A CN 200810242760A CN 200810242760 A CN200810242760 A CN 200810242760A CN 101524634 A CN101524634 A CN 101524634A
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- maize straw
- straw core
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Abstract
The invention discloses a maize straw core absorbing material and a preparing method thereof, which includes the following steps: the maize straw core is crashed to be steamed and boiled in high pressure, sucked, filtered and washed in a mixed solution comprising high boiling-point alcohol and alkali; the filtered slag is oxidized by the oxidizing agent H2O2 and rapidly cooled; the absorbing material is obtained after refrigeration and drying. The preparing method of the invention uses the maize straw core as the raw material for preparing the absorbing material which effectively absorbs neutral protease and maltogenic amylase but does not inactivate the enzyme, sufficiently uses the natural resource, simplifies the preparing method and satisfies the requirements of sustainable development.
Description
Technical field
The present invention relates to sorbing material and preparation method thereof, be specifically related to maize straw core absorbing material and preparation method thereof.
Background technology
Enzyme is as a kind of special biocatalyst, has higher selectivity and catalytic efficiency, reaction condition gentleness, catalytic activity can be regulated advantages such as control.The high activity of enzymatic reaction and the synthetic and fractionation that high selectivity carries out asymmetric syntheses, optically active compound and native compound in organic synthesis, have been utilized.But free enzyme is very responsive to environment of living in, and is all stable inadequately in strong acid, highly basic, high temperature, high ion concentration and part organic solvent, causes the sex change of zymoprotein easily, thereby reduces even lose its catalytic activity.Simultaneously, be difficult for after the free enzyme reaction separating with product with substrate, not only influence product purity but also be difficult to reuse, this has limited the extensive use of enzymatic reaction to a great extent.Enzyme immobilization technology has overcome the above-mentioned deficiency of free enzyme, improved the storage stability of enzyme, realized repeated use and continuous automatic production, reduced cost, had a wide range of applications in fields such as bioengineering, food industry, medicine and fine chemistry industry.
The performance of immobilised enzymes depends primarily on process for fixation and employed carrier material.Wherein, the performance of carrier material directly influences the catalytic activity of its immobilised enzymes.The immobilization of enzyme has very high requirement to carrier material.Desirable carrier material should possess excellent mechanical intensity, heat endurance and chemical stability, anti-biological degradability and to the high affinity of enzyme, and can keep higher enzymatic activity etc.The carrier material of therefore, design, exploitation and processability excellence has become one of emphasis of immobilised enzymes area research.
Traditional inorganic carrier material convenient sources, cheapness, mechanical strength height, nontoxic and good stability generally is to prepare immobilised enzymes by adsorption method, or prepares immobilised enzymes through little molecular chemistry modification in the covalent bonding mode.But the structure of inorganic carrier is easy-regulating not, influences the ability of mass transfer and bonding enzyme.The organic polymer carrier is one of carrier material that receives much attention in immobilised enzymes research and the application, then is the important channel that people obtain desirable Carrier Materials of Immobilized Enzyme to its modification.But this raw material need be introduced the active group that has with the enzyme effect by complicated synthetic reaction, again with the enzyme appendix from the teeth outwards on former macromolecular material.For example chemistry is circulated a notice of (Yang Yong, Li Yanfeng, visit the progress [J] of enzyme immobilization technology usefulness carrier materials such as filial piety forever, the chemistry circular, 257-262) is gone up the immobilization beta galactosidase method of introducing at 2007 the 4th phases, earlier with methyl methacrylate MMA glycerol polymerization to nylon membrane, again with the MMA glycerol polymerization to the polystyrene clad, introduced a large amount of reactive ester groups on the film surface, relend and help activation of hexamethylene diamine and glutaraldehyde and covalency.The preparation of this carrier material will be used the synthetic organic polymer material, and preparation process is quite complicated.Thereby study from resourceful natural goods, particularly reproducible natural discarded object is processed, and the preparation Carrier Materials of Immobilized Enzyme will have important economic value to making full use of the natural resources, carry out sustainable development.
Stalk is the discarded object of attached agricultural product, shows according to data, and China produces 6.2 hundred million tons of crop stalks per year, and the resource owning amount occupies first place in the world, and expects 2010 and reaches 7.26 hundred million tons.But 30% as agricultural fuel in these straws, and 25% as feed, 2～3% workmanship's sideline production raw materials for production, and 6～7% direct returning to farmland also have 35% about 2.2 hundred million tons of residue straws not to be used appropriately.And the utilization that acts as a fuel, being subjected to the influence of consumption idea and life style, stalk resource is in the situation of high flow rate, high pollution, low output fully, and considerable a part of agricultural crop straw is thrown aside or is directly burned, and does not obtain rational exploitation and utilization.
In all stalks, maize straw, wheat stalk and rice stalk account for 76% of total amount, and maize straw accounts for 50% (Cao Guoliang of three kinds of stalk amounts, open and drag for a short time, Zheng Fangcheng etc. the estimation [J] of the amount of China's Mainland stalk open incineration. resources science, 2006,28 (1): 9-13).Maize straw is made up of leaf, epidermis and cane.The stem stalk is a major part in three parts.And the stem stalk is made up of the stem skin and the core stalks of rice, wheat, etc.The big molecular structure of matter of cellulose, the lignin of maize straw stem skin has compactness and particularity, makes that it is to extract lignin and the high-purity cellulosic raw material of preparation.The hemicellulose that the wood sugar of maize straw core and glucose are formed has the sponginess of structure, can be processed into the sorbing material with absorption property.
Summary of the invention
The objective of the invention is: a kind of maize straw core absorbing material and preparation method thereof is provided, with the maize straw core is the feedstock production sorbing material, sorbing material adsorbs neutral proteinase and carbohydrase effectively, and do not make enzyme deactivation, carrier material for immobilised enzymes, make full use of the natural resources, simplify the preparation method, satisfy the sustainable development requirement.
Purpose of the present invention is realized by following technical scheme: at first, maize straw core is pulverized, in the mixed solvent mesohigh boiling of high-boiling point alcohol and alkali composition, suction filtration and washing; Then, gained filter residue oxidant H
2O
2Oxidation, cooling fast; At last, freeze drying gets sorbing material.
In the said method, described maize straw core is the residue after maize straw is removed leaf and peelled off hard coat.
In the said method, described maize straw core is crushed to 1-2.8mm.
In the said method, described high-boiling point alcohol is an ethylene glycol.
In the said method, described alkali is NaOH, KOH, NaHCO
3, Na
2CO
3, KHCO
3Or K
2CO
3Mass fraction is 2-10%.
In the said method, described mixed solvent is made up of the alcohol of 2～6 volumes and the alkali of 1 volume; The volume ratio of preferred alcohols and alkali is 4: 1.
In the said method, described maize straw core and mixed solvent carry out lixiviate according to the mixed solvent of 1g maize straw core and 10-20mL.
In the said method, described autoclaving is to carry out in autoclave, and pressure is 0.10-0.15MPa; Digestion time 20-50min, preferred 30min;
In the said method, after the described maize straw core autoclaving, through suction filtration and washing step, the washing agent of washing usefulness is a volumetric concentration 60%-80% ethanol, preferred 80% ethanol.
In the said method, oxidant is the H of mass fraction 2%-8%
2O
2, the H of 1g maize straw core washing back filter residue and 4-8mL
2O
2Stirring is placed in the autoclave behind the vapour cooking 20-40min, fast cooling; 5% of filter residue and 5mL H after the preferred 1g corncob stalks of rice, wheat, etc. washing
2O
2Mixed oxidization.
The present invention has the following advantages:
1, maize straw core absorbing material is 97% to the absorption percentage of neutral proteinase, is more than 80% to the absorption percentage of carbohydrase; Sorbing material behind the adsorptive enzyme is added by can be identical with the resolvase catalytic effect of equal quantities in the enzymatic reaction, and the sorbing material of maize straw core preparation can be used as the carrier material of immobilised enzymes, and does not make enzyme deactivation.
2, the maize straw core raw material sources are extensive, and technology is easy, complete biodegradable, environmentally safe.
The specific embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this present invention only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in art can make some nonessential improvement and adjustment according to foregoing.
Embodiment 1: the maize straw core after will removing leaf and peelling off hard coat is crushed to 1mm, take by weighing 10g, with the ethylene glycol of 70mL and mass fraction is the mixed solvent mixing that 2% 35mL NaOH forms, boiling 20min under the pressure 0.1-0.15MPa in autoclave, suction filtration is that the washing of 60% ethanol is to neutral with volumetric concentration; Gained filter residue mass fraction is 2% H
2O
240mL stirs, and the autoclave that places the bottom to fill water carries out vapour cooking 20min, cooling fast, freeze drying, the white sorbing material of puffy.
Embodiment 2: the maize straw core after will removing leaf and peelling off hard coat is crushed to 2mm, takes by weighing 10g, is 6% 30mL Na with the ethylene glycol of 120mL and mass fraction
2CO
3The mixed solvent of forming mixes, and pressure is boiling 30min under the 0.1-0.15MPa in autoclave, and suction filtration is that the washing of 70% ethanol is to neutral with volumetric concentration; Gained filter residue mass fraction is 5% H
2O
250mL stirs, and the autoclave that places the bottom to fill water carries out vapour cooking 30min, and water cools off fast, and freeze drying gets the white sorbing material of puffy.
Embodiment 3: the maize straw core after will removing leaf and peelling off hard coat is crushed to 2.8mm, takes by weighing 10g, is 10% 30mLKHCO with the ethylene glycol of 180mL and mass fraction
3The mixed solvent of forming mixes, boiling 50min under the pressure 0.1-0.15MPa in autoclave, and suction filtration is that the washing of 80% ethanol is to neutral with volumetric concentration; Gained filter residue mass fraction is 8% H
2O
280mL stirs, and the autoclave that places the bottom to fill water carries out vapour cooking 40min, cooling fast, and freeze drying gets the white sorbing material of puffy.
Application Example 1
The absorption of carbohydrase: the maize straw core absorbing material of getting 0.30g example 1 gained, the amylase that adds 30mL 1.0g/L is in the 100mL beaker, constantly stir 2min at normal temperatures, filter paper with prior enzyme through same concentrations after saturated filters, add ninhydrin and show bluish violet, this colored compound has maximum absorption wavelength under the 560nm wavelength, with the carbohydrase concentration in the solution before and after the spectrphotometric method for measuring absorption; Calculate absorption percentage ψ according to following formula: ψ %=(A.-A)/A。* 100, wherein, A.Be the absorbance of original solution, A is absorption back solution absorbency, and ψ is the absorption percentage, and the result is 82% for sorbing material at normal temperatures to the absorption percentage of carbohydrase.
The vigor of immobilized carbohydrase detects: added the 1mL starch solution in the test tube of label cleaning at 3,4 in the 5g/L carbohydrase that in No. 2 test tubes, adds 100 times of dilutions again, in No. 3 test tubes, add a little washs 3 times absorption carbohydrase with distilled water maize straw core absorbing material, behind the 2min, in three test tubes, drip same amount I again
2Solution, it is all colourless with the solution of the maize straw core absorbing material of absorption carbohydrase that the result adds Glucoamylase Solution, and the solution that does not add carbohydrase is blue.
Application Example 2
The absorption of neutral proteinase: get the 0.30g maize straw core absorbing material of example 2 gained, the neutral proteinase of 30mL 1.0g/L according to the identical method test of Application Example 1, is measured the concentration of filtrate in the 100mL beaker, calculate the absorption percentage; The result is 97% to the absorption percentage of neutral proteinase at normal temperatures.
The vigor of immobilized neutral proteinase detects: get 3 test tube numberings, in No. 3 test tubes, add a little washs 3 times absorption neutral proteinase with distilled water maize straw core absorbing material, add neutral proteinase liquid 1mL in 1 and No. 2 test tube, No. 1 pipe adds 0.4mol/L trichloroacetic acid solution 2mL immediately, makes enzyme deactivation; In 3 test tubes, add 1mL pH 7.0 again, mass fraction is 0.5% casein substrate buffer solution, rapid mixing, and put into 30 ℃ of accurate timing of water bath with thermostatic control immediately, in 2 and No. 3 test tubes, add 0.4mol/L trichloroacetic acid solution 2ml immediately behind the insulation 15min, make enzyme deactivation, cessation reaction is behind the placement 15min, filter, remove residue casein and zymoprotein sediment; Same No. 1 test tube filters at once, removes residue casein and zymoprotein sediment.Get each test tube filtrate 1mL then, move into respectively in other 3 test tubes, add 0.55mol/L sodium carbonate liquor 5ml and forint-phenol reagent 1mL again, shake up, insulation 20min observes change color; The solution of maize straw core absorbing material that the result adds neutral protein enzyme solutions and absorption neutral proteinase all is blue, and No. 1 test tube solution of inactivation is colourless at once and make neutral proteinase.
Claims (6)
1, maize straw core absorbing material is characterized in that: this sorbing material is got by the preparation of the corn stalk core stalks of rice, wheat, etc.
2, the preparation method of maize straw core absorbing material is characterized in that this method is: at first, maize straw core is pulverized, in the mixed solvent mesohigh boiling of high-boiling point alcohol and alkali composition, suction filtration and washing; Then, gained filter residue oxidant H
2O
2Oxidation, cooling fast; At last, freeze drying gets sorbing material; Described maize straw core is the residue after maize straw is removed leaf and peelled off hard coat; Described maize straw core is crushed to 1-2.8mm; Described high-boiling point alcohol is an ethylene glycol; Described alkali is NaOH, KOH, NaHCO
3, Na
2CO
3, KHCO
3Or K
2CO
3, mass fraction is 2-10%; Described mixed solvent is made up of the alcohol of 2～6 volumes and the alkali of 1 volume; Described maize straw core and mixed solvent carry out lixiviate according to 1g maize straw core and 10-21mL mixed solvent; Described autoclaving is to carry out in autoclave, and pressure is 0.10-0.15MPa, digestion time 20-50min; After the described maize straw core autoclaving, through suction filtration and washing step, the washing agent of washing usefulness is a volumetric concentration 60%-80% ethanol; Described oxidant is the H of mass fraction 2%-8%
2O
2, the H of 1g maize straw core washing back filter residue and 4-8mL
2O
2Stir, place autoclave to carry out vapour cooking 20-40min; Cooling fast after the boiling, freeze drying, the white sorbing material of puffy.
3. the preparation method of a kind of maize straw core absorbing material according to claim 2 is characterized in that: alcohol is 4: 1 with the volume ratio of alkali in the mixed solvent.
4. the preparation method of a kind of maize straw core absorbing material according to claim 2 is characterized in that: use intermixture lixiviate digestion time 30min in autoclave.
5. the preparation method of a kind of maize straw core absorbing material according to claim 2 is characterized in that: with suction filtration and washing behind the intermixture lixiviate digestion time 30min, washing agent is the ethanolic solution of volumetric concentration 80% in autoclave.
6. the preparation method of a kind of maize straw core absorbing material according to claim 2 is characterized in that: during oxidation processes, and 5% the H of 1g maize straw core washing back filter residue and 5ml
2O
2Mix.
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|---|---|---|---|
| CN2008102427608A CN101524634B (en) | 2008-12-30 | 2008-12-30 | Maize straw core absorbing material and preparing method thereof |
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| CN101524634B CN101524634B (en) | 2010-12-08 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578593A (en) * | 2012-02-20 | 2012-07-18 | 淮阴师范学院 | Corn straw core stalk dietary fiber and preparation method thereof |
| CN102603404A (en) * | 2012-03-26 | 2012-07-25 | 王真明 | Method for preparing fertilizer water-conserving block and medical dressing by using dried cornstalk core |
| CN103041786A (en) * | 2012-12-31 | 2013-04-17 | 卜迪迪 | Adsorbent |
| CN103599754A (en) * | 2013-12-13 | 2014-02-26 | 东华大学 | Biomass adsorbent for treating lead-containing wastewater and preparation and application methods thereof |
| CN115430452A (en) * | 2022-09-26 | 2022-12-06 | 吉林大学 | Nitrogen-modified biochar material and treatment method for organic polluted water body |
Family Cites Families (4)
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|---|---|---|---|---|
| US5730837A (en) * | 1994-12-02 | 1998-03-24 | Midwest Research Institute | Method of separating lignocellulosic material into lignin, cellulose and dissolved sugars |
| CN1424459A (en) * | 2002-12-17 | 2003-06-18 | 闽江学院 | Preparation of cellulose and lignin by high boiling alcohol solvent |
| CN101307159B (en) * | 2007-05-18 | 2011-06-15 | 杜昱光 | Process for preparing fibre with high adsorption capacity by using stalk as raw material |
| CN101230547B (en) * | 2008-02-26 | 2012-03-14 | 广西壮族自治区中医药研究院 | Method for preparing cellulose and carboxymethyl cethylose by wood fibre material |
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2008
- 2008-12-30 CN CN2008102427608A patent/CN101524634B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578593A (en) * | 2012-02-20 | 2012-07-18 | 淮阴师范学院 | Corn straw core stalk dietary fiber and preparation method thereof |
| CN102578593B (en) * | 2012-02-20 | 2013-09-11 | 淮阴师范学院 | Corn straw core stalk dietary fiber and preparation method thereof |
| CN102603404A (en) * | 2012-03-26 | 2012-07-25 | 王真明 | Method for preparing fertilizer water-conserving block and medical dressing by using dried cornstalk core |
| CN102603404B (en) * | 2012-03-26 | 2013-09-18 | 王真明 | Method for preparing fertilizer water-conserving block and medical dressing by using dried cornstalk core |
| CN103041786A (en) * | 2012-12-31 | 2013-04-17 | 卜迪迪 | Adsorbent |
| CN103599754A (en) * | 2013-12-13 | 2014-02-26 | 东华大学 | Biomass adsorbent for treating lead-containing wastewater and preparation and application methods thereof |
| CN103599754B (en) * | 2013-12-13 | 2015-10-28 | 东华大学 | A kind of biomass adsorbent and Synthesis and applications thereof processing lead waste water |
| CN115430452A (en) * | 2022-09-26 | 2022-12-06 | 吉林大学 | Nitrogen-modified biochar material and treatment method for organic polluted water body |
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|---|---|
| CN101524634B (en) | 2010-12-08 |
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