CN109706273A - A kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment - Google Patents
A kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment Download PDFInfo
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- CN109706273A CN109706273A CN201711010502.2A CN201711010502A CN109706273A CN 109706273 A CN109706273 A CN 109706273A CN 201711010502 A CN201711010502 A CN 201711010502A CN 109706273 A CN109706273 A CN 109706273A
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Abstract
The present invention provides a kind of methods of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment, the following steps are included: by lignocellulose biomass, phosphorus pentoxide mixing and ball milling, milled sample is mixed with water carries out hydrolysis, it carries out respectively obtaining after reaction containing sugared hydrolyzate and lignin residue, is then inoculated with saccharomyces cerevisiae into hydrolyzate and carries out alcohol fermentation.The advantages of the present invention are: promoting phosphorus pentoxide to come into full contact with lignocellulose biomass by ball milling, cellulose can be efficiently converted into monosaccharide product, reaction condition is relatively mild, and catalyst is cheap and easy to get；And containing sugared hydrolyzate without detoxification treatment can direct fermentation producing and ethanol, the process energy consumption low pollution is small, potentiality and prospect with large-scale industrial application.
Description
Technical field
The present invention relates to catalytic field and biomass as resources field, in particular to a kind of phosphorus pentoxide is catalyzed wooden fibre
The method for tieing up plain hydrolysed ferment.
Background technique
Biomass is a kind of very promising renewable resource.Biomass resource substitution is developed and used based on petroleum
Resource helps to alleviate the dependence to fossil energy, at the same can reduce fossil resource utilize on a large scale environment is brought it is huge broken
It is bad.Biomass convert to a step most important in the conversion process of fuel molecule and bulk chemical be monosaccharide acquisition.
The highest component of content is cellulose in lignocellulose-like biomass, and the glucogenic process of cellulose is to pass through water
What solution preocess was realized.Cellulose is to pass through the linear long-chain high molecular polymer that β-Isosorbide-5-Nitrae-glycosidic bond links are formed by glucose,
Glycosidic bond is closely connected by intramolecular in the supramolecular structure of cellulose and intermolecular hydrogen bonding, and catalyst is hindered to enter chain simultaneously
Make cellulose insoluble in Conventional solvents, therefore leads to the hypoergia in cellulose hydrolysis.Therefore, catalytic active site is developed
Point is close to these height, and closely β-Isosorbide-5-Nitrae-glycosidic bond catalyst system is very important, and then can pass through cellulose water
Solution obtains a large amount of cheap glucose resource.
There are two main classes for the production method of the glucose of presently relevant report, and one kind is using enzyme by biomass by hydrolyzation, separately
One kind is to utilize acid catalysis biomass by hydrolyzation.It is low and complicated that enzyme hydrolysis biomass is primarily limited to the cost of enzyme, hydrolysis efficiency
Preprocess method.The most common acid catalysis biomass hydrolysis process mainly utilizes the concentrated sulfuric acid and concentrated hydrochloric acid, almost can be
Sugar in biomass releases completely, but the separation of subsequent product and the recycling of acid still restrict these technologies
Using.Many researchers also attempt the hydrolysis using dilute sulfuric acid and dilute hydrochloric acid catalysis biomass, but only special reaction condition,
Such as high temperature and extremely short reaction time, the sugar of higher yields could be obtained.Such reaction condition is difficult in actual production
It controls, thus its economic and technical feasibility is not also high.In addition, some researchers can be with using solid acid catalysis biomass by hydrolyzation
Obtain higher monosaccharide yield, but due to after hydrolysis since the presence of lignin causes catalyst to be difficult to recycle.Therefore, it opens
The more more efficient catalyst systems of hair are extremely significant.
Summary of the invention
It is an object of the invention to solve biomass by hydrolyzation to produce sugared technical process low efficiency, economic cost height, reaction condition
Be difficult to control, separation and purification of products is difficult and the deficiencies of be easy to causeing environmental pollution, provide a kind of green high-efficient, cost is relatively low,
The technique by lignocellulose biomass by hydrolyzation saccharogenesis of easy to operate and suitable large-scale production and application.
A kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment provided by the invention, comprising the following steps:
(1) by lignocellulose-like biomass and phosphorus pentoxide ball mill grinding；
(2) lignocellulose-like biomass after ball milling is mixed with a certain amount of reaction dissolvent water, in confined conditions
Heating stirring hydrolysis for a period of time, be separated by solid-liquid separation after reaction, be separately recovered undissolved biomass solid residue and
Hydrating solution；
(3) a certain amount of potassium hydroxide adjustment pH value is added into hydrolyzate；
(4) then inoculation saccharomyces cerevisiae carries out alcohol fermentation.
The lignocellulose biomass is selected from microcrystalline cellulose, hemicellulose, stalk, straw, corncob, reed
In the true biomass and newspaper such as grass, xylose residue, furfural dregs, sugar grass, withy journey, bagasse, branches and leaves, discarded wood, sawdust
It is one or more；One of sugar grass or/and withy journey, waste paper or the cellulose-containing biological material of a variety of richnesses are useless
Gurry.
The Ball-milling Time of the wood fiber biomass is 0.5-24h；The mass ratio of milled sample and balls is 1g:
5~30g.
The mass ratio of the phosphorus pentoxide and lignocellulose-like biomass is 0.1%~20%.
Lignocellulose-like biomass after the ball milling and reaction dissolvent water quality volume ratio be body be 1g:(2~
200)mL。
The temperature of the hydrolysis is 150 DEG C~250 DEG C；The time of the hydrolysis is 5min~for 24 hours.
The OD of the cell density of the saccharomyces cerevisiae60Value are as follows: 0.2OD60~20OD60, fermentation temperature be 28-40 DEG C, hair
The ferment time is 2-120 hours.
The alkaline matter be ammonium hydroxide, sodium hydroxide, potassium hydroxide, magnesium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate,
The inorganic bases such as saleratus and inorganic basic salt, the pH of hydrolyzate is 3.5~5.5 after adjustment.
The present invention provides a kind of phosphorus pentoxides to be catalyzed lignocellulosic hydrolysed ferment method, comprising the following steps: will
Lignocellulose biomass, phosphorus pentoxide mixing and ball milling, milled sample mixed with water carry out hydrolysis, after reaction into
Row respectively obtains biomass solid hydrolysis residue and hydrolyzate, includes the monosaccharide such as glucose, xylose in hydrolyzate.Then
It is inoculated with saccharomyces cerevisiae into hydrolyzate and carries out alcohol fermentation.
The advantages of the present invention are: promoting catalyst phosphorus pentoxide and lignocellulosic biomass by ball milling
Matter comes into full contact with, and cellulose can be efficiently converted into monosaccharide product, reaction condition is relatively mild, and catalyst is cheap and easy to get；
And containing sugared hydrolyzate without detoxification treatment can direct fermentation producing and ethanol, the process energy consumption low pollution is small, has large-scale industry
The potentiality and prospect of application.
Detailed description of the invention
Fig. 1 collects sample for fermentation of furfural residues ethanol process and carries out quantification and qualification by HPLC.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.The scope of the present invention is defined by the appended claims and its equivalents.
All raw materials of the present invention, are not particularly limited its purity, and reagent used in following embodiment is commercially available.This
Invention is preferably pure using analyzing.
Qualitative and quantitative detecting instrument: high performance liquid chromatography (HPLC) is Agilent 1260, liquid-phase chromatographic column 87-H
Ion exchange column, column temperature are 65 DEG C, and refractive index detection device, detector is 50 DEG C；Mobile phase: 5Mm H2SO4, flow velocity 0.6ml/
Min, sample volume 25uL.
Comparative example 1
It weighs 2g corn stover to be placed in ball grinder, ball milling 2 hours.Then 400mg milled sample is weighed in reaction kettle,
4mL solvent is added, keep normal pressure and seals reaction kettle.Reaction kettle is placed on magnetic stirring apparatus, with the heating speed of 10 DEG C/min
Rate is warming up to 215 DEG C and maintains 40min.To after reaction, be cooled to room temperature, product liquid is collected.Determined by HPLC
Property and quantitative analysis, the result is shown in tables 1.
Comparative example 2~4
It weighs 5g corn stover furfural dregs to be placed in ball grinder, ball milling 2 hours.Then 40mg milled sample is weighed in reaction
In kettle, 4mL solvent is added, keep normal pressure and seals reaction kettle.Reaction kettle is placed on magnetic stirring apparatus, with the liter of 10 DEG C/min
Warm rate is warming up to 215 DEG C and maintains 40min.To after reaction, be cooled to room temperature, product liquid is collected.By HPLC into
Row quantification and qualification, the result is shown in tables 1.
Comparative example 5
It weighs 40mg corn stover furfural dregs to be placed in reaction kettle, 4mL solvent is added, keep normal pressure and seal reaction kettle.
Reaction kettle is placed on magnetic stirring apparatus, be warming up to 215 DEG C with the heating rate of 10 DEG C/min and maintains 40min.Wait react knot
Shu Hou is cooled to room temperature, and collects product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 1.
The composition and reaction result of system are answered in the anti-lignocellulose biomass hydrolysis of 1 comparative example of table 1~5
Embodiment 1
Weigh 5g corn stover, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then 40mg is weighed
4mL water is added in reaction kettle in milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed on magnetic stirring apparatus, with
The heating rate of 10 DEG C/min is warming up to 215 DEG C and maintains 40min.To after reaction, be cooled to room temperature, collects liquid and produce
Object.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 2
Weigh 5g corn stover, 0.5g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then 40mg is weighed
4mL water is added in reaction kettle in milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed on magnetic stirring apparatus, with
The heating rate of 10 DEG C/min is warming up to 215 DEG C and maintains 40min.To after reaction, be cooled to room temperature, collects liquid and produce
Object.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 3
Weigh 5g corn stover, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 8 hours.Then 40mg is weighed
4mL water is added in reaction kettle in milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed on magnetic stirring apparatus, with
The heating rate of 10 DEG C/min is warming up to 215 DEG C and maintains 40min.To after reaction, be cooled to room temperature, collects liquid and produce
Object.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 4
Weigh 10g corn stover furfural dregs, 0.5g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 40mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 5
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 40mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 6
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 400mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 7
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 800mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 8
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 1000mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic force to stir
It mixes on device, be warming up to 215 DEG C with the heating rate of 10 DEG C/min and maintain 40min.To after reaction, be cooled to room temperature, receive
Collect product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 9
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 200mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 50min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 10-13
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then claim
It takes 400mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 30-60min.To after reaction, be cooled to room temperature, receive
Collect product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 14
Weigh 10g corn stover furfural dregs, 1.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 4 hours.Then claim
It takes 400mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 200 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 30min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 15
Weigh 20g corn stover furfural dregs, 2.0g phosphorus pentoxide mixing be placed in ball grinder, ball milling 8 hours.Then claim
It takes 400mg milled sample in reaction kettle, 4mL water is added, keep normal pressure and seal reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 200 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 30min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 16
Weigh 2g rice husk furfural dregs, 0.2g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 40mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 205 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 30min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 17
Weigh 2g rice husk furfural dregs, 0.2g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 400mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 205 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 30min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 18
Weigh 2g rice husk furfural dregs, 0.2g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 600mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 205 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 30min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 19
Weigh 2g rice husk furfural dregs, 0.4g phosphorus pentoxide mixing be placed in ball grinder, ball milling 10 minutes.Then it weighs
4mL water is added in reaction kettle in 40mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 180 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 120min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 20
Weigh 2g rice husk furfural dregs, 0.4g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 40mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 120 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 120min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 21
Weigh 2g rice husk furfural dregs, 0.1g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 2000mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic agitation
On device, 180 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 30min.To after reaction, be cooled to room temperature, collect
Product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 22
Weigh 2g rice husk furfural dregs, 0.02g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then it weighs
4mL water is added in reaction kettle in 40mg milled sample, keeps normal pressure and seals reaction kettle.Reaction kettle is placed in magnetic stirring apparatus
On, 250 DEG C are warming up to the heating rate of 10 DEG C/min and maintain 30min.To after reaction, be cooled to room temperature, collection liquid
Body product.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 23-26
Weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then distinguish
Weigh 40,200,400,600mg milled sample in reaction kettle, 4mL water is added, normal pressure is kept simultaneously to seal reaction kettle.It will reaction
Kettle is placed on magnetic stirring apparatus, is warming up to 215 DEG C with the heating rate of 10 DEG C/min and is maintained 40min.It is cold to after reaction
But to room temperature, product liquid is collected.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 27
Weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then distinguish
40mg milled sample is weighed in reaction kettle, 4mL water is added, normal pressure is kept and seals reaction kettle.Reaction kettle is placed in magnetic force to stir
It mixes on device, be warming up to 200 DEG C with the heating rate of 10 DEG C/min and maintain 40min.To after reaction, be cooled to room temperature, receive
Collect product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 28
Weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then distinguish
40mg milled sample is weighed in reaction kettle, 4mL water is added, normal pressure is kept and seals reaction kettle.Reaction kettle is placed in magnetic force to stir
It mixes on device, be warming up to 185 DEG C with the heating rate of 10 DEG C/min and maintain 40min.To after reaction, be cooled to room temperature, receive
Collect product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
Embodiment 29
Weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours.Then distinguish
40mg milled sample is weighed in reaction kettle, 4mL water is added, normal pressure is kept and seals reaction kettle.Reaction kettle is placed in magnetic force to stir
It mixes on device, be warming up to 170 DEG C with the heating rate of 10 DEG C/min and maintain 40min.To after reaction, be cooled to room temperature, receive
Collect product liquid.Quantification and qualification is carried out by HPLC, the result is shown in tables 2.
The composition and reaction result of 2 Examples 1 to 3 of table, 8 reaction system
Embodiment 30
(1) weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours；(2) so
2400mg milled sample is weighed respectively afterwards in reaction kettle, 24mL water is added, normal pressure is kept and seals reaction kettle.Reaction kettle is set
In on magnetic stirring apparatus, 215 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to
Then room temperature carries out being separated by solid-liquid separation and collects product liquid；(3) 1.92 mMs of potassium hydroxide are added into hydrolyzate and adjust pH value
To 4.46；(4) it is inoculated with brewing yeast cell density degree 1.6*108A/mL carries out alcohol fermentation, fermentation time under the conditions of 33 DEG C
72 hours.Fermentation process collects sample and carries out quantification and qualification by HPLC, and the result is shown in Figure 1.
Embodiment 31
(1) weigh 5g Fast growth poplar furfural dregs, 0.25g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours；(2) so
3600mg milled sample is weighed respectively afterwards in reaction kettle, 24mL water is added, normal pressure is kept and seals reaction kettle.Reaction kettle is set
In on magnetic stirring apparatus, 200 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to
Then room temperature carries out being separated by solid-liquid separation and collects product liquid；(3) 1.92 mMs of potassium hydroxide are added into hydrolyzate and adjust pH value
To 4.46；(4) it is inoculated with brewing yeast cell density degree 1.0*108A/mL carries out alcohol fermentation, fermentation time under the conditions of 33 DEG C
72 hours.Fermentation process collects sample and carries out quantification and qualification by HPLC, and the result is shown in tables 3.
Embodiment 32
(1) weigh 5g rice husk furfural dregs, 0.5g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours；(2) then
4800mg milled sample is weighed respectively in reaction kettle, 24mL water is added, and is kept normal pressure and is sealed reaction kettle.Reaction kettle is placed in
On magnetic stirring apparatus, 200 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room
Then temperature carries out being separated by solid-liquid separation and collects product liquid；(3) 1.80 mMs of potassium hydroxide adjustment pH value are added into hydrolyzate extremely
4.0；(4) it is inoculated with brewing yeast cell density degree 1.0*108A/mL carries out alcohol fermentation, the fermentation time 48 under the conditions of 33 DEG C
Hour.Fermentation process collects sample and carries out quantification and qualification by HPLC, and the result is shown in tables 3.
Embodiment 33
(1) weigh 5g corn furfural dregs, 0.5g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours；(2) then
5000mg milled sample is weighed respectively in reaction kettle, 24mL water is added, and is kept normal pressure and is sealed reaction kettle.Reaction kettle is placed in
On magnetic stirring apparatus, 190 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room
Then temperature carries out being separated by solid-liquid separation and collects product liquid；(3) 1.90 mMs of potassium hydroxide adjustment pH value are added into hydrolyzate extremely
4.2；(4) it is inoculated with brewing yeast cell density degree 1.0*108A/mL carries out alcohol fermentation, the fermentation time 24 under the conditions of 33 DEG C
Hour.Fermentation process collects sample and carries out quantification and qualification by HPLC, and the result is shown in tables 3.
Embodiment 34
(1) weigh 5g corn furfural dregs, 0.5g phosphorus pentoxide mixing be placed in ball grinder, ball milling 2 hours；(2) then
4800mg milled sample is weighed respectively in reaction kettle, 24mL water is added, and is kept normal pressure and is sealed reaction kettle.Reaction kettle is placed in
On magnetic stirring apparatus, 185 DEG C are warming up to the heating rate of 10 DEG C/min and maintains 40min.To after reaction, be cooled to room
Then temperature carries out being separated by solid-liquid separation and collects product liquid；(3) 1.90 mMs of potassium hydroxide adjustment pH value are added into hydrolyzate extremely
4.3；(4) it is inoculated with brewing yeast cell density degree 1.0*108A/mL carries out alcohol fermentation, the fermentation time 48 under the conditions of 33 DEG C
Hour.Fermentation process collects sample and carries out quantification and qualification by HPLC, and the result is shown in tables 3.
Table 3: lignocellulose biomass hydrolyzate fermentation ethyl alcohol processed
| Embodiment | Ethanol yield/% | Ethyl alcohol/g.L-1 |
| 31 | 85.4 | 20.8 |
| 32 | 81.9 | 26.1 |
| 33 | 83.6 | 31.6 |
| 34 | 84.8 | 29.0 |
Claims (8)
1. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment, it is characterised in that follow the steps below:
(1) by lignocellulose-like biomass and phosphorus pentoxide mixing and ball milling；
(2) lignocellulose-like biomass after ball milling is mixed with water, one section of hydrolysis of heating stirring in confined conditions
Time is separated by solid-liquid separation after reaction, and undissolved solid biomass residue and hydrolyzate is separately recovered；
(3) alkaline matter is added into hydrolyzate and adjusts pH value；
(4) then inoculation saccharomyces cerevisiae carries out alcohol fermentation.
2. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: the lignocellulose biomass be microcrystalline cellulose, stalk, straw, corncob, alfa, xylose residue, furfural dregs,
One of sugar grass, withy journey, bagasse, branches and leaves, discarded wood, sawdust and other true biomass are a variety of；Or sweet tea
One of sorghum or/and withy journey, waste paper or the cellulose-containing biological material of a variety of richnesses or waste.
3. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: step (1) wood fiber biomass is 10min-24h with phosphorus pentoxide Ball-milling Time.
4. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: the mass ratio of step (1) phosphorus pentoxide and lignocellulose-like biomass is 0.001~0.2:1.
5. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: lignocellulose-like biomass and water solid-to-liquid ratio after described step (2) ball milling are 0.01~0.5g/mL.
6. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: the temperature of described step (2) hydrolysis is 120 DEG C~250 DEG C；The time of the hydrolysis is 5min~for 24 hours.
7. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In step (3) hydrolyzate pH adjusted be 3.5~5.5.
8. a kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment described in accordance with the claim 1, feature exist
In: the cell density of the saccharomyces cerevisiae are as follows: 0.5*108Hundred million -1.8*108A/mL, when fermentation temperature is 28-40 DEG C, ferments
Between be 2-120 hours.
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