CN109439806A - A kind of method that the Eupatorium adenophorum hydrolysis of ultrasonic microwave auxiliary prepares oligosaccharide - Google Patents
A kind of method that the Eupatorium adenophorum hydrolysis of ultrasonic microwave auxiliary prepares oligosaccharide Download PDFInfo
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- CN109439806A CN109439806A CN201811127238.5A CN201811127238A CN109439806A CN 109439806 A CN109439806 A CN 109439806A CN 201811127238 A CN201811127238 A CN 201811127238A CN 109439806 A CN109439806 A CN 109439806A
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- eupatorium adenophorum
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- 244000062748 Eupatorium adenophorum Species 0.000 title claims abstract description 81
- 229920001542 oligosaccharide Polymers 0.000 title claims abstract description 29
- 150000002482 oligosaccharides Chemical class 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 21
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000011017 operating method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 238000000855 fermentation Methods 0.000 description 4
- 230000004151 fermentation Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- NAOLWIGVYRIGTP-UHFFFAOYSA-N 1,3,5-trihydroxyanthracene-9,10-dione Chemical compound C1=CC(O)=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1 NAOLWIGVYRIGTP-UHFFFAOYSA-N 0.000 description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- -1 biogas fermentation Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 230000006854 communication Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 1
- 229940114124 ferulic acid Drugs 0.000 description 1
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 1
- 235000001785 ferulic acid Nutrition 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Sustainable Development (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses the methods that a kind of auxiliary Eupatorium adenophorum hydrolysis of ultrasonic microwave prepares oligosaccharide.Step includes: that H beta-molecular sieve is baked to 5 ~ 8h at 550 DEG C of Muffle furnace, is equally dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtains the Eupatorium adenophorum of 60 ~ 100 mesh evacuation.Eupatorium adenophorum cauline leaf after evacuation is mixed with H beta-molecular sieve, aqueous solution, in ultrasonic microwave combined reactor, using certain solid-to-liquid ratio, ultrasonic power, microwave radiation temperature, microwave power, reaction regular hour, obtains oligosaccharide solution.Oligosaccharide is produced using the method, is substantially shorter the reaction time, reduces energy consumption, it is more convenient to make operating procedure, and good hydrolysis effect can be reached.
Description
Technical field
The present invention relates to the methods that a kind of auxiliary Eupatorium adenophorum hydrolysis of ultrasonic microwave prepares oligosaccharide, belong to biomass fibre
Tie up plain resource utilization field.
Background technique
Eupatorium adenophorum (Eupatoriumadenophorum) is a kind of worldwide invasive weed, is that composite family is more
Year bunch type fruticuli herbaceous plant, originates in one band of South America Mexico to Costa Rica, has been distributed widely in generation
The boundary torrid zone, a countries and regions in subtropical zone more than 30.The protocol is passed in the 40's of 20th century by states such as Burma, India, Vietnam
Yunnan Province of China border Lincang Prefecture south, in provinces and regions such as the Yunnan of southwest, Guizhou, Sichuan, Chongqing, Guangxi, Tibet
It is widely distributed, and still with about 30 km speed every year with southwester eastwards and northwards spread in china, to local agriculture, woods,
Animal husbandry production causes serious economic loss.In recent years, domestic and foreign scholars were to Eupatorium adenophorum using having carried out more
Extensive research, including as the biological organic source of manure, biogas fermentation, insecticide processed, produce wood-based plate, make dyestuff, production xylose
Alcohol etc., but all have the defects that certain.Such as when carrying out biogas fermentation with Eupatorium adenophorum, due to contain in it umbrella shape flower ester,
Firpene, limonene, ferulic acid etc. have the activity of sterilization, disinfection, can make the micropopulation slow poisoning in biogas fermentation,
To inhibit the normal operation of biogas fermentation.Many scholars are intended to study the chemical component of Eupatorium adenophorum and the change to eciophyte
Sense effect.But the research hitherto reported in terms of resource utilization is hydrolyzed to oligosaccharide is very few.The master of Eupatorium adenophorum stalk
Ingredient holocellulose, lignin, pentosan total content is wanted to reach 85.8%, so being applied to if oligosaccharide can be hydrolyzed to
By the quantum jump to Eupatorium adenophorum resource utilization in terms of industrial alcohol production and medicine food, significant warp is improved for society
Ji and environmental benefit.
Ultrasonic wave is a kind of sound wave of the frequency higher than 20000 hertz, its good directionality, penetration capacity is strong, is easily obtained
Compared with the sound energy of concentration, propagation distance is remote in water.The mechanism of ultrasonic wave can facilitate the emulsification of liquid, the liquefaction of gel and consolidate
The dispersion of body.When forming standing wave in ultrasonic fluid medium, the molecule to suspend in a fluid is because of the effect by mechanical force
And condense upon at node, periodic accumulation is formed in space.And ultrasonic wave is in the communication process of medium, just there are one
The alternating cycles of negative pressure, in positive pressure phase, ultrasonic wave squeezes medium molecule, changes the original density of medium, makes its increasing
Greatly；In negative pressure phase, keep medium molecule sparse, further discrete, the density of medium reduces, when the ultrasound with enough large amplitudes
When wave acts on liquid medium, average distance between medium molecule can be more than the scf molecule that remains unchanged liquid medium away from
From liquid medium will be broken, and form microvesicle.These small cavities swell and are closed rapidly, can make to send out between liquid particle
Vigorous strong effect of impact, to generate thousands of pressure to a atmospheric pressure up to ten thousand.This violent interaction, meeting between particle
It increases the temperature of liquid suddenly, plays good stirring action, so that two kinds of immiscible liquid (Ru Shui and oil) be made to send out
Lactogenesis, and accelerate the dissolution of solute, accelerate chemical reaction.This various effects caused by ultrasonic wave effect in a liquid
The referred to as cavitation of ultrasonic wave.
Microwave refers to that wavelength is very short, the very high electromagnetic wave of frequency, frequency from 300MHz to 3THz, wavelength from 1m to 0.1mm,
Hydrone in heated medium material is polar molecule.It is under fast-changing electromagnetic field of high frequency (microwave) effect, pole
Sexual orientation will change with the variation of external electric field.The effect of the spin motion of hydrone is caused, the field energy of microwave field turns at this time
The thermal energy in medium is turned to, temperature of charge is increased, a series of materializing procedures such as thermalization is generated and reaches micro-wave drying
Purpose.It in biomass by hydrolyzation is that biomass by hydrolyzation is further probed by microwave applications.Microwave Pretreatment is acted in microwave irradiation
Polar molecule in raw material vibrates, and a large amount of collision frictions generate heat during violent molecular thermalmotion, and cellulose is brilliant
The molecular structure of body structure and lignocellulose raw material is destroyed, and whole crystallinity reduces.
Therefore, Eupatorium adenophorum cauline leaf cellulose family is assisted to develop hydrolysis system easy, efficiently, environmentally friendly using ultrasonic microwave
The method of standby oligosaccharide has important economic benefit and social benefit.
Summary of the invention
The present invention provides a kind of method that the Eupatorium adenophorum cauline leaf hydrolysis of ultrasonic microwave auxiliary prepares oligosaccharide, specifically includes
Step:
(1) modulation of catalyst: molecular sieve H β being placed in Muffle furnace and is baked, and cooling is spare；
(2) Eupatorium adenophorum pre-processes: being successively dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry processing, obtaining
The Eupatorium adenophorum evacuated to 60 ~ 100 mesh；
(3) ultrasonic microwave combination accessory molecule sieve H β hydrolyzes Eupatorium adenophorum: by Eupatorium adenophorum stem and leaf powder, water and the baking of evacuation
H beta-molecular sieve after roasting stirs evenly, and is placed in ultrasonic power, microwave temperature, microwave power, and the reaction time presets micro-
Wave is intracavitary, and reaction solution takes supernatant after 4000r/min is centrifuged 15min, is neutralized to neutral meta-alkalescence with NaoH solution, obtains water
Solve liquid.
Further, the H beta-molecular sieve in step 1 bakes 5-8 hours at 550 DEG C.
Further, the weight ratio of the Eupatorium adenophorum stem and leaf powder and H beta-molecular sieve evacuated in step 3 is 0.5:1 ~ 5:1,
The solid-to-liquid ratio that the Eupatorium adenophorum stem and leaf powder and water of evacuation are formed by solution is 6:1 ~ 16:1；Ultrasonic power be 200 ~
900w, 30 ~ 95 DEG C of microwave temperature, microwave power is 200 ~ 900W, and the reaction time is 5 ~ 60min；Adjust PH to neutral meta-alkalescence institute
NaoH concentration is 10%.
Beneficial effects of the present invention: present invention process is simple, and in the industrial production, saccharic acid is easily separated in product, and solid
Catalyst H β recoverable；Using ultrasonic microwave combination technique, good effect can not only be reached by pre-processing one-step hydrolysis
Fruit, and it is easy to operate, and work efficiency is high；H beta-molecular sieve requires to substantially reduce compared with anti-corrosion ability of the mineral acid hydrolysis to equipment；H
Beta-molecular sieve can carry out saccharic acid separation in the product, and catalyst reaches recycling, have to utilize in technology production and significantly drop
Low cost.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1: carrying out the hydrolysis of Eupatorium adenophorum using method as discussed in the summary of the invention section in the present embodiment, wherein
Raw material is 0.5g by evacuation treated Eupatorium adenophorum stem and leaf powder.
H beta-molecular sieve: it is baked 5 hours for 550 DEG C in Muffle furnace, purpose is easier the cellulose in lignocellulosic
The active site for contacting H beta-molecular sieve, improves the catalytic performance of catalyst.
Cutting crushes Eupatorium adenophorum: being dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtaining
The Eupatorium adenophorum of 100 mesh evacuation.
Ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: precise Eupatorium adenophorum stem and leaf powder 0.5g,
The water of 60ml is first added in container, then precise 0.5gH beta-molecular sieve stirs evenly, and is placed in microwave cavity, presetting ultrasound
Wave power 400w, 60 DEG C of microwave temperature, microwave power 500w react 10min.Reaction solution is after 4000r/min is centrifuged 15min
Supernatant is taken, PH7 ~ 9 is neutralized to 10%(w/w) NaoH solution, obtains hydrolyzate, produce oligosaccharide.By above-mentioned process
Afterwards, the conversion ratio that ultrasonic microwave combination auxiliary H β hydrolysis Eupatorium adenophorum cauline leaf prepares oligosaccharide is 58%.
Wherein H beta-molecular sieve is purchased from Catalyst Factory, Nankai Univ, and ultrasonic microwave combination ultrasonic microwave combination used is anti-
Device (combined instrument) is answered to originate from Nanjing Xian Ou instrument manufacturing Co., Ltd.
Embodiment 2: raw material is 0.5g Eupatorium adenophorum stem and leaf powder in the present embodiment；
H beta-molecular sieve: it is baked 6 hours for 550 DEG C in Muffle furnace.
Cutting crushes Eupatorium adenophorum: being dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtaining
The Eupatorium adenophorum of 100 mesh evacuation.
Ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: precise Eupatorium adenophorum stem and leaf powder 0.5g,
The water of 70ml is first added in container, then precise 0.7gH beta-molecular sieve stirs evenly, and is placed in ultrasonic power 500w, microwave
Temperature 70 C, microwave power 600w, the reaction time, 20min was preset in the microwave cavity of parameter.Reaction solution by 4000r/min from
Supernatant is taken after heart 15min, 7 ~ 9 is neutralized to 10%(w/w) NaoH solution, obtains hydrolyzate, produce oligosaccharide.
After above-mentioned process, ultrasonic microwave combination auxiliary H β hydrolysis Eupatorium adenophorum cauline leaf prepares turning for oligosaccharide
Rate is 69%.
Embodiment 3: raw material: 0.5g Eupatorium adenophorum stem and leaf powder
H beta-molecular sieve: it is baked 6 hours for 550 DEG C in Muffle furnace.
Cutting crushes Eupatorium adenophorum: being dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtaining
The Eupatorium adenophorum of 100 mesh evacuation.
Ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: precise Eupatorium adenophorum stem and leaf powder 0.5g,
The water of 80ml, then precise 1gH beta-molecular sieve are first added in container, i.e. the ratio of raw material and catalyst is 0.5:1(g/g), Gu
Liquor ratio is 6.25:1 (g/l), and solid-to-liquid ratio herein refers to the ratio of Eupatorium adenophorum raw material (g) Yu distilled water (L), and stirring is equal
It is even, it is placed in ultrasonic power 500w, 70 DEG C of microwave temperature, microwave power 600w, reaction time 20min presets the microwave of parameter
It is intracavitary.Reaction solution takes supernatant after 4000r/min is centrifuged 15min, is neutralized to 7 ~ 9 with 10%(w/w) NaoH solution, obtains water
Liquid is solved, oligosaccharide is produced.
After above-mentioned process, ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolysis Eupatorium adenophorum cauline leaf prepares oligomeric
The conversion ratio of sugar is 56%.
4 raw material of embodiment: 0.5g Eupatorium adenophorum stem and leaf powder
H beta-molecular sieve: it is baked 6 hours for 550 DEG C in Muffle furnace.
Cutting crushes Eupatorium adenophorum: being dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtaining
The Eupatorium adenophorum of 100 mesh evacuation.
Ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: precise Eupatorium adenophorum stem and leaf powder 0.5g,
The water of 80ml, then precise 0.1gH beta-molecular sieve are first added in container, i.e. the ratio of raw material and catalyst is 5:1(g/g), Gu
Liquor ratio is 6.25:1 (g/l), and solid-to-liquid ratio herein refers to the ratio of Eupatorium adenophorum raw material (g) Yu distilled water (L), and stirring is equal
It is even, it is placed in ultrasonic power 450w, 75 DEG C of microwave temperature, microwave power 700w, reaction time 20min presets the microwave of parameter
It is intracavitary.Reaction solution takes supernatant after 4000r/min is centrifuged 15min, is neutralized to 7 ~ 9 with 10%(w/w) NaoH solution, obtains water
Liquid is solved, oligosaccharide is produced.
After above-mentioned process, ultrasonic microwave combination auxiliary H β hydrolysis Eupatorium adenophorum cauline leaf prepares turning for oligosaccharide
Rate is 53%.
Embodiment 5: raw material: 0.5g Eupatorium adenophorum stem and leaf powder
H beta-molecular sieve: baking 6 hours for 550 DEG C in Muffle furnace, and purpose makes the cellulose in lignocellulosic be easier to contact H
The active site of β improves the catalytic performance of catalyst.
Cutting crushes Eupatorium adenophorum: being dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry, obtaining
The Eupatorium adenophorum of 100 mesh evacuation.
Ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: precise Eupatorium adenophorum stem and leaf powder 0.5g,
The water of 3 0ml, then precise 0.1gH beta-molecular sieve are first added in container, i.e. the ratio of raw material and catalyst is 5:1(g/g),
Solid-to-liquid ratio is 16.67:1 (g/l), and solid-to-liquid ratio herein refers to the ratio of Eupatorium adenophorum raw material (g) Yu distilled water (L), is stirred
Uniformly, it is placed in ultrasonic power 450w, 75 DEG C of microwave temperature, microwave power 700w, reaction time 20min presets the micro- of parameter
Wave is intracavitary.Reaction solution takes supernatant after 4000r/min is centrifuged 15min, is neutralized to 7 ~ 9 with 10%(w/w) NaoH solution, obtains
Hydrolyzate produces oligosaccharide.
After above-mentioned process, ultrasonic microwave combination auxiliary H β hydrolysis Eupatorium adenophorum cauline leaf prepares turning for oligosaccharide
Rate is 51%.
Embodiment 6: carrying out the hydrolysis of Eupatorium adenophorum using sulphur acid as catalyst in this example,
1, raw material: 100g Eupatorium adenophorum cauline leaf
2, sulfuric acid is deployed: the concentrated sulfuric acid being slowly added in distilled water at room temperature, 65% sulfuric acid solution is finally made into, is cooled to room
Warm standby is used.
3, it cuts, crush Eupatorium adenophorum: Eupatorium adenophorum cauline leaf being dried, is cut, is crushed, is sieved, re-dry, is obtained
The Eupatorium adenophorum of 80 mesh evacuation.
4, ultrasonic wave auxiliary pretreatment: the Eupatorium adenophorum cauline leaf after evacuation is mixed with 65% sulfuric acid solution, according to 1:4 mass
Than mixing, ultrasonic power 220w, ultrasonic 30min, at room temperature, using the Mechanical Crushing and cavitation of ultrasonic wave,
Change the coherent condition of cellulose.
5, microwave-assisted hydrolysis: by the slurries after ultrasonic pretreatment in 100 DEG C of microwave temperature, power 800w, radiation
Reaction is hydrolyzed under the conditions of 20min, prepares oligosaccharide.
After above-mentioned process, the conversion ratio that Eupatorium adenophorum cauline leaf sulphuric acid hydrolysis prepares oligosaccharide is 50%.
As can be seen from the above-described embodiment, it is used using the conversion ratio ratio that H beta-molecular sieve catalysis Eupatorium adenophorum prepares oligosaccharide
High conversion rate of the sulfuric acid as oligosaccharide prepared by catalyst.
Specific embodiments of the present invention are explained in detail above, but the present invention is not limited to above-described embodiment,
Those of ordinary skill in the art within the scope of knowledge, can also make various without departing from the purpose of the present invention
Variation.
Claims (5)
1. a kind of method that the Eupatorium adenophorum hydrolysis of ultrasonic microwave auxiliary prepares oligosaccharide, which comprises the steps of:
(1) modulation of catalyst: H beta-molecular sieve being placed in Muffle furnace and is baked, and cooling is spare；
(2) Eupatorium adenophorum pre-processes: being successively dried, cuts to Eupatorium adenophorum cauline leaf, crushing, sieving, re-dry processing, obtaining
The Eupatorium adenophorum stem and leaf powder evacuated to 60 ~ 100 mesh；
(3) ultrasonic microwave combination auxiliary H beta-molecular sieve hydrolyzes Eupatorium adenophorum: by Eupatorium adenophorum stem and leaf powder, water and the baking of evacuation
H beta-molecular sieve after roasting stirs evenly, and is placed in ultrasonic power, microwave temperature, microwave power, and the reaction time presets micro-
Wave is intracavitary, and reaction solution takes supernatant after 4000r/min is centrifuged 15min, is neutralized to neutral meta-alkalescence with NaoH solution, obtains water
Liquid is solved, oligosaccharide is produced.
2. the method that ultrasonic microwave auxiliary Eupatorium adenophorum hydrolysis according to claim 1 prepares oligosaccharide, feature exist
In the H beta-molecular sieve in the step (1) bakes 5-8 hours at 550 DEG C.
3. the method that ultrasonic microwave auxiliary Eupatorium adenophorum hydrolysis according to claim 1 prepares oligosaccharide, feature exist
In the weight ratio of the Eupatorium adenophorum stem and leaf powder and H beta-molecular sieve evacuated in the step (3) is 0.5:1 ~ 5:1, the purple of evacuation
The solid-to-liquid ratio that stem Herba Lycopi stem and leaf powder and water are formed by solution is 6:1 ~ 16:1.
4. the method that ultrasonic microwave auxiliary Eupatorium adenophorum hydrolysis according to claim 1 prepares oligosaccharide, feature exist
In ultrasonic power is 200 ~ 900w in the step (3), and 30 ~ 95 DEG C of microwave temperature, microwave power is 200 ~ 900W, reaction
Time is 5 ~ 60min.
5. the method that ultrasonic microwave auxiliary Eupatorium adenophorum hydrolysis according to claim 1 prepares oligosaccharide, feature exist
In adjusting NaoH concentration used in PH to neutral meta-alkalescence in the step (3) is 10%.
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| CN101423558A (en) * | 2008-12-17 | 2009-05-06 | 四川大学 | Eupatorium adenophorum spreng polysaccharide and preparation method and use |
| CN103013670A (en) * | 2013-01-14 | 2013-04-03 | 云南农业大学 | Microwave assisted extracted crofton weed volatile oil |
| CN103031344A (en) * | 2012-03-05 | 2013-04-10 | 朱静 | Method for degrading eupatorium adenophorum into fermentable reducing sugar |
| CN106978206A (en) * | 2017-03-29 | 2017-07-25 | 昆明理工大学 | A kind of microwave catalysis is pyrolyzed Eupatorium adenophorum production method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423558A (en) * | 2008-12-17 | 2009-05-06 | 四川大学 | Eupatorium adenophorum spreng polysaccharide and preparation method and use |
| CN103031344A (en) * | 2012-03-05 | 2013-04-10 | 朱静 | Method for degrading eupatorium adenophorum into fermentable reducing sugar |
| CN103013670A (en) * | 2013-01-14 | 2013-04-03 | 云南农业大学 | Microwave assisted extracted crofton weed volatile oil |
| CN106978206A (en) * | 2017-03-29 | 2017-07-25 | 昆明理工大学 | A kind of microwave catalysis is pyrolyzed Eupatorium adenophorum production method |
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