CN106928023A - Improve the common catalysis process of metal-enzyme preparation of the molten leaching of Salanesol in abandoned tobacco - Google Patents
Improve the common catalysis process of metal-enzyme preparation of the molten leaching of Salanesol in abandoned tobacco Download PDFInfo
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- CN106928023A CN106928023A CN201511009262.5A CN201511009262A CN106928023A CN 106928023 A CN106928023 A CN 106928023A CN 201511009262 A CN201511009262 A CN 201511009262A CN 106928023 A CN106928023 A CN 106928023A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
Abstract
A kind of common catalysis process of the metal-enzyme preparation of the molten leaching of Salanesol in raising abandoned tobacco, belongs to technical field of solanesol extraction.The present invention is with solid tobacco waste as raw material, acted on using the dual concerted catalysis of the compound enzyme and the manganese series catalyzer for improving enzyme preparation catalysis activity of catalyzing hydrolysis tobacco plant tissue, product is obtained through pretreatment of raw material, metal-enzyme preparation simple process that altogether prepared by catalytic reaction, ultrasonic synergistic treatment, Salanesol product, the dissolution rate and recovery rate of product is improved.The raw material sources of the inventive method are wide, and with twice laid fully, low production cost is simple to operate, method environmental protection, and the Salanesol product recovery rate and purity of preparation be high and the features such as complete bioactivity.The composite can be widely applied to extract the molten leaching of Salanesol, nicotine, pectin and cellulose etc. natural products from solid tobacco waste and extract, effectively realize that the resource of abandoned tobacco is recycled.
Description
Technical field
The invention belongs to technical field of solanesol extraction, and in particular to the gold of the molten leaching of Salanesol in a kind of raising abandoned tobacco
The common catalysis process of category-enzyme preparation.
Background technology
Salanesol is three sesquiterpenoids, is naturally stored in tobacco leaf（The 0.3%~3% of gross weight）, potato leaf（About 1.5% is left
It is right）, mulberry leaf（About 0.1%）In, with stronger anticancer bioactive, frequently as the important source material of pharmaceutical synthesis, it is applied to：
1. Studies on Ubiquinone Derivatives such as Co-Q10 is synthesized；2. tumor is synthesized；3. anti-ulcer medicament is synthesized；4. the heart is treated in synthesis
Cerebrovascular disease medicine；5. synthesizing anti-AIDS cytotoxic drug, has broad application prospects.Existing Salanesol extractive technique mainly has
Solvent extraction, supercritical extraction, polymeric form coprecipitation, fresh method homogenate extraction and molecular distillation technique etc., or it is many
Or effectively can promote the dissolution of natural Salanesol, but strong acid by lignocellulose degradation less（Alkali）, high temperature（Pressure）Etc. process conditions not
High energy consumption, high pollution are only resulted in, and easily makes Salanesol that addition, oxidation, dehydrogenation and molecular rearrangement reaction etc. occur, reduce resource
Utilization rate.Therefore, research improves the extracting method of Salanesol, has very important significance.
The existing method for extracting Salanesol, Publication No. CN104072336A's is " a kind of as disclosed in 1 day October in 2014
The technique for extracting Salanesol ", disclosed method is with waste/hypo-tobacco leaf as raw material, using supercritical chromatography, using overcritical two
The good selectivity of carbonoxide and the selectivity of resin, through pretreatment of raw material, one-level extraction, two grades of extractions, three-level extraction, wash-outs
Recrystallize afterwards, filter and dry, obtain Salanesol.Wherein, one-level extraction is useless secondary using the molten leaching of supercritical carbon dioxide slightly to carry
All components in tobacco leaf, raw material filling rate is 80%, and extraction temperature is 65-75 DEG C；Two grades of extractions are using adsorbent in extraction kettle
（Molecular sieve, alundum (Al2O3) or activated carbon）Dewaxing, degreasing and removal of impurities are completed, temperature is 60-70 DEG C；Three-level extraction is utilized to be had
The chromatography silica gel or resin of selectivity complete the absorption of Salanesol, and are eluted using ethyl acetate or petroleum ether, and it is 95% to obtain purity
Salanesol.The major defect of the method is：（1）The method utilizes the molten leaching solanesol in tobacco leaves of supercritical carbon dioxide,
But the dissolution of other components in tobacco leaf is also enhanced simultaneously, because the diversity of dissolution component increases Impurity removal difficulty, therefore is adopted
Three-level extraction process is taken, and then is increased manufacturing facilities, increase production cost；（2）The method three-level extraction each stage takes difference
The adsorbent of function, increases raw materials for production, increases production cost；（3）Used with adsorption function in two grades of extractions of the method
Molecular sieve, alundum (Al2O3) or activated carbon are adsorbent, though completing dewaxing, degreasing and removal of impurities, can also adsorb Salanesol, are reduced
The recovery rate of Salanesol, lowers production yields in three-level extraction；（4）The method is produced need to use supercritical technology, and during
Extraction temperature is higher than 60 DEG C, not only needs special production equipment, also needs external heat source equipment, further increases production cost.
The content of the invention
The purpose of the present invention is, for the deficiency of existing extraction Salanesol method, there is provided one kind improves eggplant in abandoned tobacco
Metal-the enzyme preparation of the molten leaching of Buddhist nun's alcohol catalysis process altogether, with reaction condition it is gentle, operating procedure is few and simple, the molten leaching of Salanesol
Fully and impurity is few, energy consumption and the features such as low cost.
Mechanism of the invention is：The present invention with abandoned tobacco as raw material, from engineering enzyme（Zytase：Cellulase：Paint
Enzyme）It is the activator of enzyme preparation as the enzyme preparation of catalytic activation lignocellulosic, manganese series catalyzer, by zytase and paint
The lignin of yoke cellulose in enzyme degrading tobacco, increases hydrolysis of the cellulase to cellulose, by metallic catalyst
The catalysis activity of enzyme preparation is improved, enhancing hinders the hydrolysis degree of the tobacco plant fibr tissue of Salanesol dissolution, improves plant
Tissue permeability, reduces Salanesol resistance to mass tranfer, increases Salanesol recovery rate.The two concerted catalysis hydrolysed tobacco string group
Knit, because of the selectivity of enzyme, reduce the dissolution of other active components in tobacco leaf, while chemical activating agent acid, the usage amount of alkali are avoided,
Reduce Salanesol production safety hidden danger, it is to avoid the secondary pollution that soda acid is caused using increasing to environment, be conducive to environmental protection,
Realize that abandoned tobacco resource is recycled.
Realizing the technical scheme of goal of the invention is：Metal-the enzyme preparation of the molten leaching of Salanesol is common in a kind of raising abandoned tobacco
Catalysis process, with abandoned tobacco as raw material, processed through pretreatment of raw material, the common catalytic reaction of metal-enzyme preparation, ultrasonic synergistic,
Salanesol product prepares product.Methods described is comprised the following steps that：
（1）Pretreatment of raw material
With solid tobacco waste（It is always natural including the leftover bits and pieces in waste/hypo-tobacco leaf, offal, tobacco processing course and extraction tobacco
Scarp of product etc.）It is raw material.After first starting material with water is cleaned up, it is positioned in baking oven, first in 85~110 DEG C of baking oven
Dry 30~90min, then after size-reduced machine is crushed and cross 20~120 mesh sieves, unsifted raw material is crushed again in returning to pulverizer,
Collect sieving raw material（As pretreated raw material）.
（2）The common catalytic reaction of metal-enzyme preparation
The（1）After the completion of step, first according to the（1）Material quality (g) after step treatment: catalyst quality (g): the volume of water
The ratio between (ml) for 1: 0.0125~0.075: 5~15 ratio, the（1）In walking pretreated raw material, add catalyst and
Water, after stirring, then is 4~8 with the pH value of sulfuric acid or dilute solution of sodium hydroxide regulation system, then by after regulation pH value
Mixed liquor is positioned in shaking table, and enzymolysis 4~8h of activation is carried out at being 20~45 DEG C in bath temperature, and suction filtration is carried out with suction filter pump,
Filtrate and filter residue are collected respectively.The filtrate of collection is the aqueous extract containing Salanesol；The filter residue of collection is to be urged through catalyst
Change the tobacco base-material after activation.Described catalyst is the metal-enzyme preparation of metal and compound enzyme, and the ratio between its dosage is metal
Catalyst（g）: enzyme preparation（g）=1:1.6~10；Described metal is manganese-zinc ferrite（Mn0.3Zn0.2Fe0.5Ox）Or Mn2+Or
Fe3+；The enzyme preparation is that enzyme activity ratio is zytase：Cellulase：Laccase=2~14: 23~47: 51~64 compound enzyme.
（3）Ultrasonic synergistic treatment
The（2）After the completion of step, first by（2）The filter residue collected is walked, i.e. tobacco base-material is transferred in leaching vessel, according still further to the
（1）The quality (g) of raw material after step pretreatment: the ratio between volume (ml) of compound extracting agent solution is 1: 8~12 ratio, is being soaked
Carry and compound extracting agent solution is added in container, be uniformly mixed, and in 30~55 DEG C of 100~200W of ultrasonic power, temperature
Under the conditions of carry out 5~40min of ultrasonication after, carry out suction filtration with suction filtration machine, respectively collect filtrate and filter residue.Filter to collecting
Slag is used as the raw material for preparing sorbing material；The filtrate of collection is transferred in centrifuge, is 3000~4000r/min in centrifugal rotational speed
Under the conditions of, after being centrifuged 10~40min, centrifugal clear liquid is collected respectively（As contain the extract solution of Salanesol）And centrifugation
Slag.Centrifugation slag to collecting is transferred to the（2）Filter residue in step, as the raw material for preparing sorbing material；Centrifugal clear liquid to collecting leads to
The concentration of high effective liquid chromatography for measuring Salanesol is crossed, i.e., by the mobile phase ethanol of high performance liquid chromatography: the volume ratio of methyl alcohol
It is 1: 4~9 ratio, is 0.6~1.2ml/min in flow velocity, under the conditions of 20~30 DEG C of column temperature, in the centrifugal clear liquid that measure is collected
Salanesol mass concentration and dissolution rate.Salanesol dissolution rate is 92.00~98.70%, and dissolution rate improves 15.00~24.90%.
Described compound extracting agent solution is ethanol: the mass concentration ratio of methyl alcohol is 1: 1~9 ethanol and the mixed liquor of methyl alcohol.
（4）It is prepared by Salanesol product
The（3）After the completion of step, first by（3）Walk the centrifugal clear liquid collected to be positioned in a rotary evaporator, in vacuum pressure
For 0.1~0.6Mpa, temperature are at 30~60 DEG C, be concentrated under reduced pressure into thick Salanesol semifinished product.Then, according to eggplant
The quality (g) of Buddhist nun's alcohol semifinished product: the ratio between volume (ml) of compound collecting agent solution is 1: 3~6 ratio, in leaching vessel
Salanesol crude product and compound extracting agent solution are added, mixed dissolution is uniform.Finally, by rotary evaporator, it is in vacuum pressure
0.1~0.6Mpa, temperature are obtained Salanesol product at 30~60 DEG C, to carry out repetition concentrated under reduced pressure 2~4 times.Salanesol is extracted
Rate is up to 90.0~97.5%, high purity 91.0~94.0%%.
The present invention is after adopting the above technical scheme, mainly have the following effects：
（1）The present invention, as the collaboration activator of catalytic activation lignocellulosic, improves eggplant from metallic catalyst and compound enzyme
The recovery rate of Buddhist nun's alcohol.Again through metal-enzyme preparation concerted catalysis degrading tobacco lignocellulosic, the biology that can improve enzyme preparation is living
Property, and then tobacco internal permeability is improved, and Salanesol dissolution resistance to mass tranfer is reduced, promote the molten leaching of Salanesol abundant, therefore, this hair
Bright method gained Salanesol dissolution rate is 98.64%, and 24.90% is improved than ultrasonic alcohol extracting method, and its recovery rate is up to 97.3%.
（2）The present invention replaces traditional chemical activator soda acid to extract Salanesol and nicotine with metal-enzyme preparation, reduces soda acid
Destruction Deng chemical reagent to Salanesol bioactivity, interfering component is less in its leaching liquor, and bioactivity retains complete, can be really
Protect product quality.Replace activator soda acid with enzyme, while avoiding the corrosion of acid-base pair production equipment in production process and shortening
Production equipment service life, is conducive to environmental protection, and production cost is reduced again.
（3）The solid tobacco waste that the present invention is used is through enzyme（Cellulase or lignin or cellulase and lignin
Enzyme compound enzyme）Catalytic activation condition is optimal at 20~40 DEG C, and enzymolysis time is only 7.5 hours, and reaction condition is gentle, operation letter
It is single, and the organic solvent that extraction Salanesol is used is methyl alcohol and ethanol, reduces high temperature or a large amount of toxic organic solvents extract eggplant Buddhist nun
The production safety hidden danger of alcohol, in reduction production process while environment treatment cost, improves production safety performance, and energy is reduced again
Consumption.
（4）The raw material sources of the inventive method are wide, and fully, low production cost is simple to operate for twice laid, method green ring
Protect.The inventive method can be widely applied to solid tobacco waste for raw material obtains through refining Salanesol, be also widely applied to from solid
The extraction of nicotine, pectin, cellulose in tobacco waste.
Specific embodiment
With reference to specific embodiment, the present invention is further described.
Embodiment 1
A kind of metal-the enzyme preparation of the molten leaching of Salanesol in raising abandoned tobacco is total to comprising the following steps that for catalysis process：
（1）Pretreatment of raw material
The tobacco leaf that 40g is discarded is cleaned, after drying, is positioned in baking oven, taken out after drying 30min in 100 DEG C of baking oven, through powder
Broken machine crosses the sieve screening of 60 molecules of interest after crushing, obtain tobacco leaf of the particle diameter less than 60 mesh, is dispensed with polybag, standby.
（2）The common catalytic reaction of metal-enzyme preparation
The（1）After the completion of step, first according to the（1）Material quality (g) after step treatment: catalyst quality (g): the volume of water
The ratio between (ml) for 1: 0.035: 10 ratio, the（1）Walk in pretreated raw material, add catalyst and water, stir
Afterwards, then with the pH value of sulfuric acid or dilute solution of sodium hydroxide regulation system it is 7, then the mixed liquor adjusted after pH value is positioned over and is shaken
In bed, enzymolysis activation 7.5h is carried out at being 45 DEG C in bath temperature, suction filtration is carried out with suction filter pump, filtrate and filter residue are collected respectively.
The filtrate of collection is the aqueous extract containing Salanesol；The filter residue of collection is the tobacco base-material after being activated through catalyst.
Described catalyst is the metal-enzyme preparation of metal and compound enzyme, and the ratio between its dosage is metallic catalyst（g）: enzyme preparation（g）
=1:5；Described metal is manganese-zinc ferrite Mn0.3Zn0.2Fe0.5Ox；The enzyme preparation is that enzyme activity ratio is zytase：Cellulose
Enzyme：Laccase=14: 23: 63 compound enzyme.
（3）Ultrasonic synergistic treatment
The（2）After the completion of step, first by（2）The filter residue collected is walked, i.e. tobacco base-material is transferred in leaching vessel, according still further to the
（1）The quality (g) of raw material after step pretreatment: the ratio between volume (ml) of compound extracting agent solution is 1: 10 ratio, is being extracted
Compound extracting agent solution is added in container, is uniformly mixed, and surpassed under the conditions of ultrasonic power 200W, temperature 50 C
After sonicated 25min, suction filtration is carried out with suction filtration machine, filtrate and filter residue are collected respectively.Filter residue to collecting is adsorbed as preparation
The raw material of material；The filtrate of collection is transferred in centrifuge, under the conditions of centrifugal rotational speed is 4000r/min, is centrifuged
After 15min, centrifugal clear liquid is collected respectively（As contain the extract solution of Salanesol）With centrifugation slag.Centrifugation slag to collecting is transferred to the
（2）Filter residue in step, as the raw material for preparing sorbing material；Centrifugal clear liquid to collecting passes through high effective liquid chromatography for measuring eggplant Buddhist nun
The concentration of alcohol, i.e., in the mobile phase ethanol of high performance liquid chromatography: the volume ratio of methyl alcohol is 1: 6 ratio, is in flow velocity
0.8ml/min, under the conditions of 25 DEG C of column temperature, determines the Salanesol mass concentration and dissolution rate in the centrifugal clear liquid collected.Salanesol
Dissolution rate is 98.64%, and dissolution rate improves 24.9%.Described compound extracting agent solution is ethanol: the mass concentration ratio of methyl alcohol is 1
: 5.5 ethanol and the mixed liquor of methyl alcohol.
（4）It is prepared by Salanesol product
The（3）After the completion of step, first by（3）Walk the centrifugal clear liquid collected to be positioned in a rotary evaporator, in vacuum pressure
For 0.2Mpa, temperature are at 45 DEG C, be concentrated under reduced pressure into thick Salanesol semifinished product.Then, it is rough according to Salanesol
The quality (g) of product: the ratio between volume (ml) of compound collecting agent solution is 1: 5 ratio, adds Salanesol thick in leaching vessel
Product and compound extracting agent solution, mixed dissolution are uniform.Finally, it is that 0.2Mpa, temperature are in vacuum pressure by rotary evaporator
At 45 DEG C, be concentrated under reduced pressure is repeated 3 times, and Salanesol product is obtained.Salanesol extraction rate reached 97.3%, high purity 93.5%.
Embodiment 2
A kind of method of the common catalysis process of the metal-enzyme preparation of the molten leaching of Salanesol in raising abandoned tobacco, with embodiment 1, wherein：
The（1）It is 20 mesh from tobacco mesh number in step, oven temperature is 85 DEG C, and drying time is 90min.
The（2）In step, the quality (g) of solid tobacco waste: catalyst quality (g): the ratio between volume (ml) of water is 1:
0.0125: 5 ratio.The pH value for using hydrochloric acid solution regulation system is 4, and enzymolysis bath temperature is 25 DEG C.Enzymolysis activation tobacco
Base-material 8h.The ratio between described metal-enzyme preparation dosage is metallic catalyst（g）: enzyme preparation（g）=1:1.6；The enzyme preparation
For enzyme activity ratio is zytase：Cellulase：Laccase=2: 47: 51 compound enzyme.
The（3）In step, the quality of pretreated solid tobacco waste: composite extractant liquor capacity ratio is 1:8, it is multiple
Close extractant ethanol: the volume ratio of methyl alcohol is 1: 1.Ultrasonic power is 200W, ultrasonic temperature is 30 DEG C, and ultrasonic time is 5
min；Filtrate centrifuge RPMs are 4000r/min, and centrifugation time is 25min.High performance liquid chromatography mobile phase ethanol and methyl alcohol
Volume ratio is 1: 9, and flow velocity is 1.2ml/min, and column temperature is 30 DEG C.Salanesol dissolution rate is 92.03%, and dissolution rate is improved
16.56%。
The（4）In step, suction filtration vacuum pressure is 0.6Mpa, thickening temperature is 60 DEG C.The quality (g) of Salanesol semifinished product:
The ratio between volume (ml) of compound collecting agent solution is 1: 3.Salanesol extraction rate reached 95.9%, purity is up to 91.5%.
Embodiment 3
A kind of method of the common catalysis process of the metal-enzyme preparation of the molten leaching of Salanesol in raising abandoned tobacco, with embodiment 1, wherein：
The（1）It is 120 mesh from tobacco mesh number in step, oven temperature is 110 DEG C, and drying time is 30min.
The（2）In step, the quality (g) of solid tobacco waste: catalyst quality (g): the ratio between volume (ml) of water is 1:
0.075: 15 ratio.The pH value for using hydrochloric acid solution regulation system is 6, and bath temperature is 45 DEG C.Enzymolysis activation tobacco base-material
4h.The ratio between described metal-enzyme preparation dosage is metallic catalyst（g）: enzyme preparation（g）=1:10；The enzyme preparation is enzyme activity
Than being zytase：Cellulase：Laccase=2: 34: 64 compound enzyme.
The（3）In step, the quality of pretreated solid tobacco waste: composite extractant liquor capacity ratio is 1:12,
Composite extractant ethanol: the volume ratio of methyl alcohol is 1: 9.Ultrasonic power is 100W, ultrasonic temperature is 55 DEG C, and ultrasonic time is
40 min；Filtrate centrifuge RPMs are 3000r/min, and centrifugation time is 10min.High performance liquid chromatography mobile phase ethanol and methyl alcohol
Volume ratio be 1: 4, flow velocity is 0.6ml/min, and column temperature is 20 DEG C.Salanesol dissolution rate is 95.30%, and dissolution rate is improved
20.7%。
The（4）In step, suction filtration vacuum pressure is 0.1Mpa, thickening temperature is 30 DEG C.The quality (g) of Salanesol semifinished product:
The ratio between volume (ml) of compound collecting agent solution is 1: 6.Salanesol extraction rate reached 93.2%, purity is up to 92.0%.
Experimental result
1st, using the molten comparing for soaking Salanesol of method and other method of embodiment 1
Table 1 obtains through refining the comparing of Salanesol product and compounding enzymatic hydrolysis and ultrasonic alcohol extracting method
| Method | Concentration（mg/ml） | Molten leaching rate（%） | Molten extraction high rate（%） | Recovery rate（%） | Purity（%） | Organic solvent usage amount（ml） | Reaction temperature（℃） | Extraction time（min） |
| Metal-enzyme preparation solution technique | 0.1794 | 98.64 | 24.90 | 97.30 | 93.50 | 20 | 45 | 30 |
| Compounding enzymatic hydrolysis | 0.1687 | 92.76 | 17.49 | 92.80 | 91.0 | 20 | 45 | 30 |
| Ultrasonic alcohol extracting | 0.1435 | 78.95 | __ | 78.95 | 75.60 | 50 | 50th, heat | 50 |
Know from above-mentioned experiment：Using metal-enzyme, catalytic activation treatment solid tobacco waste prepares activated carbon to the present invention altogether, works as throwing
Plus with solid tobacco leaf waste material amount ratio be 1：0.035 enzyme（Zytase：Cellulase：Laccase activity ratio is 14: 23:
63）, it is 1 to add water volume ratio：10,45 DEG C under the nearly room temperature condition of water-bath, enzymolysis time is 7.5h, is cooperateed with through compound extractant
It is ultrasonically treated that Salanesol product is obtained, while accessory substance nicotine can be obtained.Wherein tobacco enzymolysis activates base-material quality (g): multiple
It is 1 to close the ratio between extractant liquor capacity (ml):10, compound extractant ethanol：The volume ratio of methyl alcohol is 1: 5.5, ultrasonic wave work(
Rate is 200W, ultrasonic temperature is 50 DEG C, and ultrasonic extraction time is 25 min.Fully, its molten leaching rate is the dissolution of the method Salanesol
98.64%, improve 24.90% than ultrasonic alcohol extracting method.The method enzyme replaces soda acid activator, and preparation condition is gentle, not only avoids
The corrosion of acid-base pair production equipment, and the production safety hidden danger that high temperature prepares product is reduced, simple to operate, Salanesol product is carried
Take rate and purity is high, and bioactivity is complete, while reducing soda acid and harmful organic substance in production process are caused to environment two
Secondary pollution, is conducive to environmental protection, reduces production cost.
Claims (4)
1. a kind of metal-enzyme preparation for improving the molten leaching of Salanesol in abandoned tobacco is total to catalysis process, it is characterised in that methods described
Comprise the following steps that：
（1）Pretreatment of raw material
With solid tobacco waste as raw material, including the leftover bits and pieces in waste/hypo-tobacco leaf, offal, tobacco processing course and extraction tobacco
Scarp of total natural products etc., after first starting material with water is cleaned up, is positioned in baking oven, first in 85~110 DEG C of baking oven
Dry 30~90min, then after size-reduced machine is crushed and cross 20~120 mesh sieves, unsifted raw material is crushed again in returning to pulverizer,
Collect sieving raw material（As pretreated raw material）；
（2）The common catalytic reaction of metal-enzyme preparation
The（1）After the completion of step, first according to the（1）Material quality after step treatment: catalyst quality: the ratio between volume of water is 1g
: the ratio of 0.0125~0.075 g: 5~15ml,（1）Walk in pretreated raw material, add catalyst and water, stirring
After uniform, then it is 4~8 with the pH value of sulfuric acid or dilute solution of sodium hydroxide regulation system, then will adjusts the mixed liquor after pH value
It is positioned in shaking table, enzymolysis 4~8h of activation is carried out at being 20~45 DEG C in bath temperature, suction filtration is carried out with suction filter pump, receives respectively
Collection filtrate and filter residue, the filtrate of collection is the aqueous extract containing Salanesol, and the filter residue of collection is to be activated through catalyst
Tobacco base-material afterwards, described catalyst is metal and the metal-enzyme preparation of compound enzyme, and the ratio between its dosage is metallic catalyst
: enzyme preparation=1 g:1.6~10 g；Described metal is manganese-zinc ferrite（Mn0.3Zn0.2Fe0.5Ox）Or Mn2+Or Fe3+；The enzyme
Preparation is that enzyme activity ratio is zytase：Cellulase：Laccase=2~14: 23~47: 51~64 compound enzyme；
（3）Ultrasonic synergistic treatment
The（2）After the completion of step, first by（2）The filter residue collected is walked, i.e. tobacco base-material is transferred in leaching vessel, according still further to the
（1）The quality of raw material after step pretreatment: the ratio between volume of compound extracting agent solution is the ratio of 1 g: 8~12 ml, in extraction
Compound extracting agent solution is added in container, is uniformly mixed, and in 100~200W of ultrasonic power, 30~55 DEG C of bars of temperature
After carrying out 5~40min of ultrasonication under part, suction filtration is carried out with suction filtration machine, filtrate and filter residue are collected respectively, to the filter residue collected
As the raw material for preparing sorbing material；The filtrate of collection is transferred in centrifuge, is 3000~4000r/min bars in centrifugal rotational speed
Under part, after being centrifuged 10~40min, centrifugal clear liquid is collected respectively（As contain the extract solution of Salanesol）With centrifugation slag,
Centrifugation slag to collecting is transferred to the（2）Filter residue in step, as the raw material for preparing sorbing material；Centrifugal clear liquid to collecting passes through height
Effect liquid phase chromatogram method determines the concentration of Salanesol, i.e., by the mobile phase ethanol of high performance liquid chromatography: the volume ratio of methyl alcohol is 1: 4
~9 ratio, is 0.6~1.2ml/min in flow velocity, under the conditions of 20~30 DEG C of column temperature, determines the eggplant in the centrifugal clear liquid collected
Buddhist nun's alcohol mass concentration and dissolution rate, Salanesol dissolution rate are 92.00~98.70%, dissolution rate raising 15.00~24.90%, described
Compound extracting agent solution be ethanol: the mass concentration ratio of methyl alcohol for 1: 1~9 ethanol and methyl alcohol mixed liquor；
（4）It is prepared by Salanesol product
The（3）After the completion of step, first by（3）Walk the centrifugal clear liquid collected to be positioned in a rotary evaporator, in vacuum pressure
For 0.1~0.6Mpa, temperature are at 30~60 DEG C, be concentrated under reduced pressure into thick Salanesol semifinished product, then, according to eggplant
The quality of Buddhist nun's alcohol semifinished product: the ratio between volume of compound collecting agent solution is the ratio of 1 g: 3~6ml, adds in leaching vessel
Salanesol crude product and compound extracting agent solution, mixed dissolution are uniform, finally, by rotary evaporator, vacuum pressure be 0.1~
0.6Mpa, temperature are obtained Salanesol product, Salanesol extraction rate reached at 30~60 DEG C, to carry out repetition concentrated under reduced pressure 2~4 times
90.0~97.5%, high purity 91.0~94.0%%.
2. a kind of metal-enzyme preparation for improving the molten leaching of Salanesol in abandoned tobacco according to claim 1 is total to catalysis process,
It is characterized in that：
The（1）It is 60 mesh from abandoned tobacco mesh number in step, oven temperature is 100 DEG C, and drying time is 30min；
The（2）In step, solid tobacco waste quality: catalyst quality: the ratio between volume of water is 1 g: 0.035 g: 10 ml,
Solution ph is 7, and enzymolysis bath temperature is 45 DEG C, and enzymolysis time is 7.5h, manganese-zinc ferrite in catalyst: enzyme preparation=1 g: 5
G, enzyme preparation enzyme activity ratio is zytase：Cellulase：Laccase=14: 23: 63；
The（3）In step, the quality of pretreated solid tobacco waste: composite extractant liquor capacity ratio is 1:10, it is combined
Extractant ethanol: the volume ratio of methyl alcohol is 1: 5.5, ultrasonic power is 200W, and ultrasonic temperature is 50 DEG C, and ultrasonic time is 25
min；Filtrate centrifuge RPMs are 4000r/min, and centrifugation time is 15min, high performance liquid chromatography mobile phase ethanol and methyl alcohol
Volume ratio is 1: 6, and flow velocity is 0.8ml/min, and column temperature is 25 DEG C, and Salanesol dissolution rate is 98.64%, and dissolution rate is improved
24.9%；
The（4）In step, suction filtration vacuum pressure is 0.2Mpa, thickening temperature is 45 DEG C, the quality of Salanesol semifinished product: compound collecting
The ratio between volume of agent solution is 1 g: 5 ml, Salanesol extraction rate reached 97.3%, and purity is up to 93.5%.
3. a kind of metal-enzyme preparation for improving the molten leaching of Salanesol in abandoned tobacco according to claim 1 is total to catalysis process,
It is characterized in that：
The（1）It is 20 mesh from tobacco mesh number in step, oven temperature is 85 DEG C, and drying time is 90min；
The（2）In step, the quality of solid tobacco waste: catalyst quality: the ratio between volume of water is 1: 0.0125 g: 5 ml's
Ratio, the pH value for using hydrochloric acid solution regulation system is 4, and bath temperature is 25 DEG C, enzymolysis activation tobacco base-material 8h, described gold
The ratio between category-enzyme preparation dosage is metallic catalyst: enzyme preparation=1 g:1.6 g；The enzyme preparation is that enzyme activity ratio is xylan
Enzyme：Cellulase：Laccase=2: 47: 51 compound enzyme；
The（3）In step, the quality of pretreated solid tobacco waste: composite extractant liquor capacity ratio is 1:8, it is combined extraction
Take agent ethanol: the volume ratio of methyl alcohol is 1: 1, ultrasonic power is 200W, ultrasonic temperature is 30 DEG C, and ultrasonic time is 5 min；
Filtrate centrifuge RPMs are 4000r/min, and centrifugation time is the volume of 25min, high performance liquid chromatography mobile phase ethanol and methyl alcohol
Ratio is 1: 9, and flow velocity is 1.2ml/min, and column temperature is 30 DEG C, and Salanesol dissolution rate is 92.03%, and dissolution rate improves 16.56%；
The（4）In step, suction filtration vacuum pressure is 0.6Mpa, thickening temperature is 60 DEG C, the quality (g) of Salanesol semifinished product: compound
The ratio between the volume (ml) for extracting agent solution is 1: 3, Salanesol extraction rate reached 95.9%, and purity is up to 91.5%.
4. a kind of metal-enzyme preparation for improving the molten leaching of Salanesol in abandoned tobacco according to claim 1 is total to catalysis process,
It is characterized in that：
The（1）It is 120 mesh from tobacco mesh number in step, oven temperature is 110 DEG C, and drying time is 30min；
The（2）In step, the quality of solid tobacco waste: catalyst quality: the ratio between volume of water is 1 g: 0.075 g: 15 ml
Ratio, the pH value for using hydrochloric acid solution regulation system is 6, and bath temperature is 45 DEG C, enzymolysis activation tobacco base-material 4h, and metal urges
Agent: enzyme preparation=1g:10 g；The enzyme preparation is that enzyme activity ratio is zytase：Cellulase：Laccase=2: 34: 64 compounding
Enzyme；
The（3）In step, the quality of pretreated solid tobacco waste: composite extractant liquor capacity ratio is 1:12, it is combined
Extractant ethanol: the volume ratio of methyl alcohol is 1: 9, ultrasonic power is 100W, ultrasonic temperature is 55 DEG C, and ultrasonic time is 40
min；Filtrate centrifuge RPMs are 3000r/min, and centrifugation time is 10min, high performance liquid chromatography mobile phase ethanol and methyl alcohol
Volume ratio is 1: 4, and flow velocity is 0.6ml/min, and column temperature is 20 DEG C, and Salanesol dissolution rate is 95.30%, and dissolution rate is improved
20.7%；
The（4）In step, suction filtration vacuum pressure is 0.1Mpa, thickening temperature is 30 DEG C, the quality of Salanesol semifinished product: compound collecting
The ratio between volume of agent solution is 1 g: 6 ml, Salanesol extraction rate reached 93.2%, and purity is up to 92.0%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816050A (en) * | 2012-09-13 | 2012-12-12 | 王星敏 | Method for extracting solanesol by activating waste and defective tobacco by enzyme catalysis |
| CN103014099A (en) * | 2012-12-27 | 2013-04-03 | 山东大学 | Method for promoting hydrolysis of lignocellulose |
| WO2014009749A1 (en) * | 2012-07-13 | 2014-01-16 | Kind Consumer Limited | Process for using tobacco |
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2015
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014009749A1 (en) * | 2012-07-13 | 2014-01-16 | Kind Consumer Limited | Process for using tobacco |
| CN102816050A (en) * | 2012-09-13 | 2012-12-12 | 王星敏 | Method for extracting solanesol by activating waste and defective tobacco by enzyme catalysis |
| CN103014099A (en) * | 2012-12-27 | 2013-04-03 | 山东大学 | Method for promoting hydrolysis of lignocellulose |
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