CN101792495A - Method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws - Google Patents
Method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws Download PDFInfo
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- CN101792495A CN101792495A CN 201010109597 CN201010109597A CN101792495A CN 101792495 A CN101792495 A CN 101792495A CN 201010109597 CN201010109597 CN 201010109597 CN 201010109597 A CN201010109597 A CN 201010109597A CN 101792495 A CN101792495 A CN 101792495A
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- 239000010902 straw Substances 0.000 title claims abstract description 77
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229920002678 cellulose Polymers 0.000 title claims abstract description 32
- 239000001913 cellulose Substances 0.000 title claims abstract description 32
- 229920005610 lignin Polymers 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 36
- 239000011941 photocatalyst Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 19
- 230000001699 photocatalysis Effects 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims description 47
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 17
- 238000007146 photocatalysis Methods 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000011258 core-shell material Substances 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 41
- 239000000835 fiber Substances 0.000 description 17
- 240000008042 Zea mays Species 0.000 description 15
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 15
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 15
- 235000005822 corn Nutrition 0.000 description 15
- 235000013311 vegetables Nutrition 0.000 description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 241000209140 Triticum Species 0.000 description 7
- 235000021307 Triticum Nutrition 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000002657 fibrous material Substances 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 108010059892 Cellulase Proteins 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 244000046109 Sorghum vulgare var. nervosum Species 0.000 description 3
- 229940106157 cellulase Drugs 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
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- 229920001131 Pulp (paper) Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000012978 lignocellulosic material Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
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- 238000002525 ultrasonication Methods 0.000 description 1
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Abstract
The invention discloses a method for ultrasonically catalyzing and extracting hemicellulose, cellulose and lignin from plant straws. The method comprises the following steps of: (1) airing plant straws and then mechanically crushing, collecting plant straw powder, fully drying and removing moisture; (2) dispersing the dried plant straw powder into a water solution and then carrying out ultrasonic treatment, dissolving the hemicellulose into the water solution, then separating the water solution, and carrying out photocatalytic decomposition on the separated plant straw residuals by taking nano Fe3O4-TiO2 as a photocatalyst with a core-shell structure; (3) separating and extracting lignin from the residuals subjected to the photocatalytic decomposition by using an organic solvent in an extraction way, wherein the extracted residuals are a mixture of the cellulose and the photocatalyst; and (4) putting the extracted residuals under a magnetic field to separate the cellulose from the photocatalyst to obtain the cellulose. The invention successfully realizes the separation and the full utilization of the hemicellulose, the cellulose and the lignin in the plant straws and improves the utilization ratio of renewable resources.
Description
Technical field:
The present invention relates to from the method for plant straw ultrasonically catalyzing and extracting hemicellulose, Mierocrystalline cellulose and xylogen.The pretreatment process that belongs to organic chemistry plant straw.
Background technology
People see the unprecedented challenge that we faced more and more significantly, promptly satisfy growing energy demand and protection environment.As leading on the earth and regenerated vegetable fibre resource is noticeable naturally every year.The vegetable fibre resource mainly contains agricultural crop straw and forestry waste material two big classes, and the annual stalk raw materials enormous amount that produces of China has 1,000,000,000 tons more than according to estimates approximately.These resources fail to be utilized effectively mostly, on behalf of a continuable way, vegetable fibre is converted into Industrial products satisfy the growing fuel and the demand of Chemicals, especially in view of the limited mineral wealth of supply, petroleum resources reduce day by day and to the concern of environment.
At present, extract these three kinds of main chemical compositions from vegetable fibre efficiently and remain a difficult problem as the starting material of high added value.This is owing to the chemical structure of vegetable fibre complexity and is difficult to the product that technology is difficult for obtaining enough productive rates and commercial value are arranged.For example in paper industry, the value of hemicellulose and xylogen does not obtain enough utilizations, has only about 40% material to reclaim with utilizable form.The separating technology of many lignocellulosic materials that are used for production of cellulosic ethanol is all ignored other of xylogen may purposes, and just suggestion is burned its and reclaimed heat energy.These produce the pattern of single bulk product owing to do not make full use of plant fiber material, cause low in economic efficiency, thereby limited the development of related industries.Biorefinery is similar to refining of petroleum, it is the process of each component of comprehensive utilization plant fiber material, a series of high value added product is produced in, classification processed by plant fiber material, conversion, biorefinery is a kind of approach that gets a good chance of, and makes the vegetable fibre industry have more commercial appeal.Yet for a long time, traditional plant fiber extracting mode generally adopts strong acid and strong base technology, not only the energy consumption height, pollute greatly, and extraction yield is low, causes the resource serious waste.Therefore, be necessary to set up an easy industrialized technological process.Three main components of vegetable fibre are separated separately, reduced the degraded of hemicellulose, xylogen to greatest extent, and make it become domestic and international focus the vegetable fibre comprehensive utilizating research with useful form recovery.
The main component of plant straw mainly is to be made of Mierocrystalline cellulose, hemicellulose, three kinds of components of xylogen.The hemicellulose of cross bracing and the complex body of xylogen are a kind of matrix material of cellulosic fibre formation glued together, i.e. lignocellulose.The method of three main components of general separating plant fiber mainly contains two kinds of biological process and chemical methods.Biological process mainly is to utilize cellulase that fibrous material is changed into available sugar, further is used for producing products such as lactic acid.But,, thereby hindered cellulase hydrolysis vegetable fibre material industrially scalable because enzymic hydrolysis ubiquity hydrolysis rate is slowly at present, efficient is not high and restricted by multiple factor, causes the enzymic hydrolysis cost too high.The chemistry rule is to utilize certain chemical reagent vegetable fibre to be handled under certain condition, utilizes the difference of three main component chemical property of vegetable fibre progressively to separate.But these methods generally need high temperature, high pressure, reaction extraction conditions harshness, and the use of organic solvent also easily causes the pollution of environment, uncomfortable industrialization promotion and production.Therefore, make full use of three main components in the vegetable fibre, particularly reach the standard of medicinal or foodstuff additive, be necessary to research and develop the technology and the technology of a kind of pollution-free, low-consumption high-efficiency separated fiber element, hemicellulose, xylogen.
Summary of the invention
The object of the present invention is to provide a kind of production technique simple, with low cost, use wide, be convenient to the method that realizes that large-scale industrial is produced from plant straw ultrasonically catalyzing and extracting hemicellulose, Mierocrystalline cellulose and xylogen.
For achieving the above object, the present invention has fully utilized ultrasonic wave and nano-TiO
2Premium properties.Ultrasonic wave is as a kind of method that can at room temperature inject energy, in fields such as physics, biology, chemistry, be widely used in recent years, the microjet that mechanical effect that ultrasonic wave produces in water medium and cavitation produce produces the straw surface and impacts, shears, and the heat that cavatition produced and free radical all can make macromolecules degradation.Once there are some researches show with ultrasonication Mixed Office WasteMOW and sulfate pulp, the discovery ultrasonic wave can be opened cellulosic crystallizing field, can make the morphological structure and the ultrastructure generation considerable change of wood pulp cellulose, highly beneficial to the accessibility and the chemical reaction performance that improve cellulase.In addition, under the rayed of certain energy, the photosensitive semiconductor nano-TiO
2Be inspired electron-hole pair, and that the water molecules that is adsorbed on semiconductor surface is accepted light induced electron-hole is right, thereby a series of redox reaction takes place, these reactions can disconnect between the xylogen with Mierocrystalline cellulose between be connected, can disconnect simultaneously the key of Mierocrystalline cellulose inside, reaction process does not relate to the chemical substance of any contaminate environment yet.The present invention is just at comprehensive utilization ultrasonic wave and nano-TiO
2The basis of premium properties on, what exploitation made new advances extracts the method for hemicellulose, Mierocrystalline cellulose and xylogen from vegetable fibre.
The present invention realizes that the technical scheme that its purpose is taked is:
The present invention mainly comprises the steps: from the method for plant straw ultrasonically catalyzing and extracting hemicellulose
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, and sift out and collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, collects the hemicellulose aqueous solution wherein, and hemicellulose aqueous solution drying treatment is obtained the hemicellulose solid.
Further, the present invention in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
Further, the present invention describedly obtains the hemicellulose solid with hemicellulose aqueous solution drying treatment and is to use freeze-drying or boulton process in step (2).
The present invention mainly comprises the steps: from the method that plant straw ultrasonically catalyzing extracts xylogen
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, and sift out and collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, and the plant straw residue that separation is obtained is to have the nanometer Fe of " nuclear-shell " structure
3O
4@TiO
2Photocatalyst carries out photocatalysis Decomposition;
(3) residue after the photocatalysis Decomposition is with an organic solvent gone out wherein xylogen by extractive mode separation and Extraction.
Further, the present invention in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
Further, the present invention in described step (2), nanometer Fe
3O
4@TiO
2The particle diameter of particle is 30-50nm; Wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10-30nm.
Further, when the present invention carried out described photocatalysis Decomposition in step (2), light-catalysed temperature was that 20-50 ℃, time are 30-60 minute.
The present invention extracts cellulosic method from plant straw ultrasonically catalyzing and mainly comprises the steps:
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, and the plant straw residue that separation is obtained is to have the nanometer Fe of " nuclear-shell " structure
3O
4@TiO
2Photocatalyst carries out photocatalysis Decomposition;
(3) residue after the photocatalysis Decomposition is with an organic solvent gone out wherein xylogen by extractive mode separation and Extraction, the residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst;
(4) residue after the extracting is placed Mierocrystalline cellulose is separated with photocatalyst, obtain Mierocrystalline cellulose.
Further, the present invention in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
Further, the present invention in described step (2), nanometer Fe
3O
4@TiO
2The particle diameter of particle is 30-50nm; Wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10-30nm.
The used plant straw of the present invention can in corn stalk, Chinese sorghum straw, wheat straw, paddy stalk, rape straw, the wood chip any one or any two more than.
The present invention can use 200～400 mesh sieves to collect and obtain the plant stalk powder end.
The present invention when the residue after the photocatalysis Decomposition is gone out wherein xylogen by extractive mode separation and Extraction, used organic solvent can in methyl alcohol, ethanol, ethylene glycol, propylene glycol, butyleneglycol, phenols, ketone, tetrahydrofuran (THF), the benzene class solution any or wantonly more than 2 kinds.
The present invention at the plant straw residue that separation is obtained to have the nanometer Fe of " nuclear-shell " structure
3O
4@TiO
2When photocatalyst carried out photocatalysis Decomposition, the light that is adopted can be that optical wavelength is the high voltage mercury lamp of 365nm.
Compared with prior art, advantage of the present invention is:
(1) the present invention has greatly reduced the possibility that environmental pollution produces owing to adopted ultrasonic, catalysis technique;
(2) the present invention realizes that successfully with the hemicellulose in the plant straw, Mierocrystalline cellulose and xylogen separately, each is made full use of, and further improves the utilization ratio of renewable resource.
(3) method of the present invention is simple, can reduce cost and energy consumption, is convenient to commercial scale production.
Description of drawings
Fig. 1 for the present invention from plant straw ultrasonically catalyzing and extracting hemicellulose, Mierocrystalline cellulose and and the technical process summary view of xylogen.
Embodiment
Embodiment 1:
(1) earlier corn stalk is dried, after with the corn stalk mechanical disintegration, and cross 200 mesh sieves and collect the corn stalk powder, with collected corn stalk powder thorough drying, to remove moisture.
(2) taking by weighing collected dry corn stalk powder 0.50g is dispersed in the aqueous solution that 40mL concentration is the pH=4 that regulates of the HCl of 1M and carries out supersound process, and to control ultrasonic temperature be that 40 minutes, ultrasonic power are 200 watts, ultrasonic frequency 20KHz at 30 ℃, ultrasonic time, hemicellulose in the corn stalk is dissolved in the aqueous solution, by separating, collect the hemicellulose aqueous solution, the lyophilize of the hemicellulose aqueous solution is handled obtaining hemicellulose solid 0.08g.
(3) previous step is separated the straw residue 10mg nanometer Fe that obtains
3O
4@TiO
2(wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10nm) carry out photocatalysis Decomposition (optical wavelength is 365nm) under the photocatalyst effect.Light-catalysed temperature is 50 ℃, 30 minutes time.
(4) residue after the previous step photochemical catalysis is extracted lignin separation by extractive mode with ethanol, get xylogen 0.11g after the removal ethanol drying.
(5) residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst, can separate the final Mierocrystalline cellulose 0.30g that gets of vacuum-drying under certain externally-applied magnetic field with photocatalyst fully.
Embodiment 2:
(1) after wheat straw dries in elder generation,, and crosses 200 mesh sieves and collect the wheat straw powder,, remove moisture collected wheat straw powder thorough drying with the wheat straw mechanical disintegration.
(2) taking by weighing collected drying wheat straw powder 0.50g is dispersed in the water of certain 40mL pH=7 and carries out supersound process, and control ultrasonic temperature at 40 ℃, ultrasonic time 30 minutes, 200 watts of ultrasonic powers, ultrasonic frequency 20KHz, hemicellulose in the wheat straw is dissolved in the aqueous solution, by separating, collect the hemicellulose aqueous solution, hemicellulose aqueous solution rotary evaporation is dewatered after hemicellulose solid 0.06g is arrived in vacuum-drying.
(3) previous step is separated the straw residue 10mg nanometer Fe that obtains
3O
4@TiO
2(wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10nm) carry out photocatalysis Decomposition (optical wavelength is 365nm) under the photocatalyst effect.Light-catalysed temperature is 20 ℃, 30 minutes time.
(4) residue after the previous step photochemical catalysis is extracted lignin separation by extractive mode with acetone, get xylogen 0.09g behind the removal acetone drying.
(5) residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst, can separate the final Mierocrystalline cellulose 0.31g that gets of vacuum-drying under certain externally-applied magnetic field with photocatalyst fully.
Embodiment 3:
(1) earlier rape straw is dried, after with the rape straw mechanical disintegration, and cross 400 mesh sieves and collect the rape straw powder, with collected rape straw powder thorough drying, remove moisture.
(2) taking by weighing the collected dry rape straw powder 0.50g NaOH that to be dispersed in certain 40mL concentration be 1M regulates in the aqueous solution of pH=10 and carries out supersound process, and control ultrasonic temperature at 50 ℃, ultrasonic time 20 minutes, 400 watts of ultrasonic powers, ultrasonic frequency 25KHz, hemicellulose in the rape straw is dissolved in the aqueous solution, by separating, collect the hemicellulose aqueous solution, the lyophilize of the hemicellulose aqueous solution is handled obtaining hemicellulose solid 0.11g.
(3) previous step is separated the straw residue 10mg nanometer Fe that obtains
3O
4@TiO
2(wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 20nm) carry out photocatalysis Decomposition (optical wavelength is 365nm) under the photocatalyst effect.Light-catalysed temperature is 50 ℃, 60 minutes time.
(4) residue after the previous step photochemical catalysis is extracted lignin separation by extractive mode with toluene, get xylogen 0.10g after the removal toluene drying.
(5) residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst, can separate the final Mierocrystalline cellulose 0.27g that gets of vacuum-drying under certain externally-applied magnetic field with photocatalyst fully.
Embodiment 4:
(1) earlier corn stalk is dried, after with plant straw mechanical disintegration, and cross 400 mesh sieves and collect the corn stalk powder, with collected plant stalk powder end thorough drying, remove moisture.
(2) taking by weighing collected dry corn stalk powder 0.50g is dispersed in certain 40mL water and carries out supersound process, and control ultrasonic temperature 50 ℃, ultrasonic time 60 minutes,, 500 watts of ultrasonic powers, ultrasonic frequency 25KHz, hemicellulose in the corn stalk is dissolved in the aqueous solution, by separating, collect the hemicellulose aqueous solution, the lyophilize of the hemicellulose aqueous solution is handled obtaining hemicellulose solid 0.10g.
(3) previous step is separated the straw residue 10mg nanometer Fe that obtains
3O
4@TiO
2(wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 20nm) carry out photocatalysis Decomposition (optical wavelength is 365nm) under the photocatalyst effect.Light-catalysed temperature is 20 ℃, 60 minutes time.
(4) residue after the previous step photochemical catalysis is extracted lignin separation by extractive mode with tetrahydrofuran (THF), get xylogen 0.12g after the removal tetrahydrofuran (THF) drying.
(5) residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst, can separate the final Mierocrystalline cellulose 0.25g that gets of vacuum-drying under certain magnetic field with photocatalyst fully.
Embodiment 5:
(1) earlier corn stalk and Chinese sorghum straw are dried, after with plant straw mechanical disintegration, and cross 400 mesh sieves and collect the corn stalk powder, with collected plant stalk powder end thorough drying, to remove moisture.
(2) taking by weighing collected dry corn stalk and each 0.25g of Chinese sorghum straw powder respectively is dispersed in certain 40mL water and carries out supersound process, and control ultrasonic temperature at 50 ℃, ultrasonic time 30 minutes, 800 watts of ultrasonic powers, ultrasonic frequency 25KHz, hemicellulose in the corn stalk is dissolved in the aqueous solution, by separating, collect the hemicellulose aqueous solution, hemicellulose aqueous solution rotary evaporation is dewatered after vacuum-drying obtains hemicellulose solid 0.12g.
(3) previous step is separated the straw residue 10mg nanometer Fe that obtains
3O
4@TiO
2(wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 30nm) carry out photocatalysis Decomposition (optical wavelength is 365nm) under the photocatalyst effect.Light-catalysed temperature is 20 ℃, 60 minutes time.
(4) residue after the previous step photochemical catalysis is extracted lignin separation by extractive mode with phenol, get xylogen 0.14g after the removal phenol drying.
(5) residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst, can separate the final Mierocrystalline cellulose 0.22g that gets of vacuum-drying under certain magnetic field with photocatalyst fully.
Claims (10)
1. the method from plant straw ultrasonically catalyzing and extracting hemicellulose is characterized in that comprising the steps:
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, and sift out and collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, collects the hemicellulose aqueous solution wherein, and hemicellulose aqueous solution drying treatment is obtained the hemicellulose solid.
2. according to the described method of claim 1 from plant straw ultrasonically catalyzing and extracting hemicellulose, its feature in: in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
3. according to the described method of claim 1 from plant straw ultrasonically catalyzing and extracting hemicellulose, its feature in: in step (2), describedly hemicellulose aqueous solution drying treatment obtained the hemicellulose solid be to use freeze-drying or boulton process.
4. the method from plant straw ultrasonically catalyzing extraction xylogen is characterized in that comprising the steps:
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, and sift out and collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, and the plant straw residue that separation is obtained is to have the nanometer Fe of " nuclear-shell " structure
3O
4@TiO
2Photocatalyst carries out photocatalysis Decomposition;
(3) residue after the photocatalysis Decomposition is with an organic solvent gone out wherein xylogen by extractive mode separation and Extraction.
5. according to the described method of extracting xylogen from plant straw ultrasonically catalyzing of claim 4, its feature in: in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
6. according to the described method of claim 4, it is characterized in that from plant straw ultrasonically catalyzing extraction xylogen: in described step (2), nanometer Fe
3O
4@TiO
2The particle diameter of particle is 30-50nm; Wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10-30nm.
7. extract the method for xylogen according to claim 4 is described from plant straw ultrasonically catalyzing, it is characterized in that: when carrying out described photocatalysis Decomposition in step (2), light-catalysed temperature is that 20-50 ℃, time are 30-60 minute.
8. one kind is extracted cellulosic method from plant straw ultrasonically catalyzing, it is characterized in that comprising the steps:
(1) earlier the plant straw is dried, after with plant straw mechanical disintegration, collect the plant stalk powder end, with collected plant stalk powder end thorough drying to remove moisture;
(2) dried plant stalk powder end is dispersed in carries out supersound process in the aqueous solution, hemicellulose in the plant straw is dissolved in the aqueous solution, separate the aqueous solution back, and the plant straw residue that separation is obtained is to have the nanometer Fe of " nuclear-shell " structure
3O
4@TiO
2Photocatalyst carries out photocatalysis Decomposition;
(3) residue after the photocatalysis Decomposition is with an organic solvent gone out wherein xylogen by extractive mode separation and Extraction, the residue after the extracting is the mixture of Mierocrystalline cellulose and photocatalyst;
(4) residue after the extracting is placed Mierocrystalline cellulose is separated with photocatalyst, obtain Mierocrystalline cellulose.
9. extract cellulosic method according to claim 8 is described from plant straw ultrasonically catalyzing, its feature in: in described step (2), the pH=4-10 of aqueous solutions employed when carrying out described supersound process, ultrasonic temperature is that 30-50 ℃, ultrasonic time are that 20-60 minute, ultrasonic power are that 200-800 watt, ultrasonic frequency are 20～25KHz.
10. extract cellulosic method according to claim 8 is described from plant straw ultrasonically catalyzing, it is characterized in that: in described step (2), nanometer Fe
3O
4@TiO
2The particle diameter of particle is 30-50nm; Wherein, nanometer Fe
3O
4Be nuclear, this nanometer Fe
3O
4Particle diameter be 20nm; TiO
2Be shell, this TiO
2Thickness be 10-30nm.
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