CN109337946A - A method of Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive - Google Patents
A method of Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive Download PDFInfo
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Abstract
The present invention provides a kind of method for improving Heating Explosion Sugarcane Bagasse efficiency by two stages pretreatment and additive.High-temperature-hot-water pretreatment, dilute acid pretreatment, alkali alcohol pre-treatment, enzymatic hydrolysis including Bagasse Material and etc..Smashed Bagasse Material will be air-dried to mix with high-temperature-hot-water or dilution heat of sulfuric acid, 20~40min is reacted at 100~130 DEG C carries out first segment pretreatment, it will obtain the pretreatment residue rich in cellulose and lignin, then lignin is removed through second segment alkali/alcohol pre-treatment, obtain rich cellulose-containing pretreatment residue, then cellulase and additive are added into residue and is digested, enzymolysis efficiency is improved.The present invention adds additive by two stages pretreatment and in enzymatic hydrolysis section, improves enzymolysis efficiency and reduces the dosage of cellulase, shortens enzymolysis time, save the cost has a good application prospect.
Description
Technical field
The present invention relates to a kind of methods biomass efficient conversion and utilized, more particularly, to Bagasse Material through two sections of pre- places
The method that reason and additive improve Heating Explosion Sugarcane Bagasse efficiency.
Background technique
Shortage with the energy and continuous protrusion the problems such as environment, biomass can as can be converted into liquid fuel
Regenerated resources are just paid more and more attention.On earth in biomass resource abundant, with wooden fine fiber biomass liquid
Fuel is most paid close attention to by people.
The method of wood fiber biomass preparing liquid fuel is that hemicellulose, the cellulose in the raw material are hydrolyzed into wood
The monosaccharide such as sugar, glucose, by fermentative production of ethanol, or by catalyzing and synthesizing the liquid fuels such as fuel oil.But due to biomass original
Cellulose in material is closely joined together with hemicellulose and lignin, and stable structure is not easy to be destroyed by cellulase, therefore is needed
It is pre-processed.Preprocess method used at present has high-temperature-hot-water pretreatment, acid system pretreatment, alkaline process to locate in advance
Reason, organic solvent pretreatment and ionic liquid pretreatment.These pretreatments are beaten by degradation part hemicellulose and/or lignin
It breaks it and is formed by reticular structure, improve the accessibility of cellulase, and then improve enzymolysis efficiency.These preprocess methods are independent
Although usually requiring higher pretreatment temperature, time, Yi Jihua using glucose yield in subsequent enzymolysis process can be improved
Product dosage, therefore searching is mild, efficient preprocess method is very urgent.
Although different preprocess methods can effectively improve subsequent enzymolysis efficiency, if it is logical to obtain higher enzymolysis efficiency
Higher cellulase dosage and longer enzymolysis time are often needed, the production cost of glucose is increased, therefore compels to be essential
Seek a kind of glucose production method that can be improved enzymolysis efficiency and reduce cost.
Summary of the invention
The present invention provides a kind of by two stages pretreatment and additive to overcome at least one defect in the prior art
The method for improving Heating Explosion Sugarcane Bagasse efficiency.The present invention is a kind of efficient, mild preprocess method, can pass through two stages pretreatment group
It closes and improves the conversion ratio that the biomass materials such as bagasse prepare glucose.And enzymolysis efficiency is improved by the addition of enzymatic hydrolysis section additive
While reduce and cellulase dosage and shorten enzymolysis time, to reduce the production cost of glucose.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A method of Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive, wherein the following steps are included:
S1. Bagasse Material and a certain amount of distilled water or 1% sulfuric acid solution are placed in closed reactor, 100~130
20~40min is reacted at DEG C and carries out first segment pretreatment, separates to obtain first segment pretreatment residue；
S2. a certain amount of first segment pretreatment residue and a certain amount of alkali ethyl alcohol are placed in closed reactor, 100~
40~80min is reacted at 130 DEG C and carries out second segment pretreatment, separates to obtain second segment pretreatment residue；
S3. the resulting pretreatment residue of a certain amount of step S1 and step S2 is taken respectively, and acetic acid-sodium acetate is added to it
Buffer, cellulase and additive, are digested, inactivation, and are measured to concentration of glucose；
Preferably, in the step S1, the Bagasse Material is part remaining after squeezing sugar from the sugarcane that sugar refinery obtains,
It crushes and obtains after air-drying.
Preferably, in the step S1, the mass volume ratio of the Bagasse Material and distilled water or 1% sulfuric acid solution is
1:8~15.
Preferably, in the step S2, alkali concentration is 0.3~0.6% in the alkali ethanol pre-treatment process, ethanol/water
Liquor capacity ratio is 50/50~70/30.
Preferably, described to be separated into vacuum filtration or centrifugation in the step S1 and step S2.
Preferably, in the step S3, the enzyme digestion reaction time is 6~72 hours, and temperature is 45~55 DEG C, and revolving speed is
100~200 revs/min, the pH of buffer is 4.5~6.0, and the dosage of cellulase and additive is exhausted relative to residue after pretreatment
Dry mass is respectively 10~20FPU/ grams and 100~200 milligrams per grams.
Preferably, in the step S3, the inactivation treatment that 5~15min is carried out to it is needed after the completion of the enzymolysis process.
Preferably, in the step S3, the measuring method for carrying out glucose concentration determination is high-efficient liquid phase technique.
Preferably, in the step S3, the additive is Tween 80.
Compared with prior art, the present invention has the advantage that as follows with effect:
A kind of method improving Heating Explosion Sugarcane Bagasse efficiency by two stages pretreatment and additive provided by the invention can take off step by step
Except hemicellulose and lignin, the influence of lignin and hemicellulose to enzymolysis efficiency is reduced, the efficiency of enzymatic hydrolysis is tentatively improved.Separately
Outside, method provided by the invention also joined additive in enzymolysis process, when the addition of additive greatly shortens enzymatic hydrolysis
Between, and enzyme dosage can be reduced, further improve enzymolysis efficiency；Enzymolysis efficiency improves the production that can be effectively reduced glucose
Cost.
Specific embodiment
The present invention will be further specifically described in detail with reference to specific embodiments, but embodiments of the present invention are not
It is limited to this, for not specifically specified technological parameter, can refer to routine techniques progress.
Bagasse Material used is derived from sugar refinery, its partial size < 1 millimeter after air-dried, thread rolling, pulverization process, and constituent content is
Cellulose 41.2%, hemicellulose 22.8%, lignin 25.2%.
Glucose content is analyzed with high-efficient liquid phase technique in enzymolysis liquid, and the calculation method of yield is as follows:
Y indicates glucose yield in pre- enzymolysis liquid (gram/100 grams of raw materials) in formula；C indicates concentration of glucose in enzymolysis liquid
(g/L)；V indicates enzymolysis liquid volume (L)；M indicates the quality (g) of cellulose in Bagasse Material.
Embodiment 1
It weighs 100 grams of over dry Bagasse Materials to be placed in the closed reactor equipped with thermocouple, 1000 milliliters of distilled water is added,
Stirring is opened, heating makes that temperature rapid increase to 120 DEG C and starts timing, when reaching 30 minutes in the reaction time, stop heating,
And so that reaction is down to room temperature with condensed water immediately, first segment pretreatment residue is isolated using the method for vacuum filtration.
It takes the first segment high-temperature-hot-water of 50 grams of over dry to pre-process residue to be placed in the closed reactor equipped with thermocouple, be added
500 milliliter of 60% ethanol/water solution and 2.5 grams of NaOH, open stirring, and heating makes that temperature rapid increase to 120 DEG C and starts to count
When, when reaching 60 minutes in the reaction time, stop heating, and so that reaction is down to room temperature with condensed water immediately, using vacuum filtration
Method isolate second segment alkali alcohol pre-treatment residue.
5 grams of (in terms of over dry) first segment high-temperature-hot-water pretreatment residues and second segment alkali alcohol pre-treatment residue are taken respectively,
It is separately added into acetic acid-sodium acetate of the pH=4.8 of the cellulase (match two generation of power) of 100FPU, 0.75 gram of Tween 80 and 250mL
Buffer solution is digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.Enzymatic hydrolysis takes out after carrying out 24 hours
1mL enzymolysis liquid simultaneously carries out 10min inactivation treatment, is respectively 22.8% with concentration of glucose yield in efficient liquid phase measurement enzymolysis liquid
With 69.2%.10min inactivation treatment is taken out and carried out after enzymatic hydrolysis carries out 72 hours, enzymatic hydrolysis is separated using the method for vacuum filtration
Liquid and enzymatic hydrolysis residue, with concentration of glucose in efficient liquid phase measurement enzymolysis liquid, calculating gained glucose yield is respectively 26.0%
With 71.4%.
Embodiment 2
The present embodiment is similar to Example 1, and difference is, takes 5 grams of (in terms of over dry) second segment alkali alcohol pre-treatments residual
Slag, acetic acid-sodium acetate that the pH=4.8 of the cellulase (match two generation of power) of 50FPU, 0.75 gram of Tween 80 and 250mL is added are slow
Solution is rushed to be digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.It is taken out after enzymatic hydrolysis carries out 72 hours
And 10min inactivation treatment is carried out, using the method separation enzymolysis liquid and enzymatic hydrolysis residue of vacuum filtration, is measured and digested with efficient liquid phase
Concentration of glucose in liquid, calculating gained glucose yield is 68.0%.
Other raw material dosages and operating procedure are same as Example 1.
Embodiment 3
It weighs 100 grams of over dry Bagasse Materials to be placed in the closed reactor equipped with thermocouple, 1000 milliliters of 1%H is added2SO4
Solution opens stirring, and heating makes that temperature rapid increase to 120 DEG C and starts timing, when reaching 30 minutes in the reaction time, stops
Heating, and so that reaction is down to room temperature with condensed water immediately, the pretreatment of first segment dilute sulfuric acid is isolated using the method for vacuum filtration
Residue.
It takes the first segment dilute sulfuric acid of 50 grams of over dry to pre-process residue to be placed in the closed reactor equipped with thermocouple, be added
500 milliliter of 60% ethanol/water solution and 2.5 grams of NaOH, open stirring, and heating makes that temperature rapid increase to 120 DEG C and starts to count
When, when reaching 60 minutes in the reaction time, stop heating, and so that reaction is down to room temperature with condensed water immediately, using vacuum filtration
Method isolate second segment alkali alcohol pre-treatment residue.
5 grams of (in terms of over dry) first segment dilute sulfuric acid pretreatment residues and second segment alkali alcohol pre-treatment residue are taken respectively, point
Not Jia Ru the cellulase (match two generation of power) of 100FPU, 0.75 gram of Tween 80 and 250mL pH=4.8 acetic acid-sodium acetate it is slow
Solution is rushed to be digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.Enzymatic hydrolysis takes out after carrying out 24 hours
1mL enzymolysis liquid simultaneously carries out 10min inactivation treatment, is respectively 59.0% with concentration of glucose yield in efficient liquid phase measurement enzymolysis liquid
With 69.3%.10min inactivation treatment is taken out and carried out after enzymatic hydrolysis carries out 72 hours, enzymatic hydrolysis is separated using the method for vacuum filtration
Liquid and enzymatic hydrolysis residue, with concentration of glucose in efficient liquid phase measurement enzymolysis liquid, calculating gained glucose yield is respectively 70.9%
With 76%.
Embodiment 4
The present embodiment is similar to Example 3, and difference is, takes 5 grams of (in terms of over dry) second segment alkali alcohol pre-treatments residual
Slag, acetic acid-sodium acetate that the pH=4.8 of the cellulase (match two generation of power) of 50FPU, 0.75 gram of Tween 80 and 250mL is added are slow
Solution is rushed to be digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.It is taken out after enzymatic hydrolysis carries out 72 hours
And 10min inactivation treatment is carried out, using the method separation enzymolysis liquid and enzymatic hydrolysis residue of vacuum filtration, is measured and digested with efficient liquid phase
Concentration of glucose in liquid, calculating gained glucose yield is 62.6%.
Other raw material dosages and operating procedure are same as Example 3.
Comparative example 1
Comparative example 1 is similar to Example 1, and difference is, 5 grams of (in terms of over dry) first segment high-temperature-hot-waters is taken to locate in advance respectively
Residue and second segment alkali alcohol pre-treatment residue are managed, the pH in cellulase (match two generation of power) and 250mL of 100FPU is separately added into
=4.8 acetic acid-sodium acetate buffer solution is digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.Enzyme
10min inactivation treatment is taken out and carried out to solution after carrying out 72 hours, separates enzymolysis liquid and enzymatic hydrolysis residue using the method for vacuum filtration,
With concentration of glucose in efficient liquid phase measurement enzymolysis liquid, calculating gained glucose yield is respectively 22.0% and 66%.
Other raw material dosages and operating procedure are same as Example 1.
Comparative example 1 compared with Example 1, in the comparable situation of glucose yield, the addition of Tween 80 in enzymolysis process
Enzymolysis time be can be shortened to 24 hours.Enzymatic hydrolysis condition is identical, when enzymolysis time is 72 hours, Tween 80 is added and does not add tween
80 first segment high-temperature-hot-water pretreatment residue is compared with glucose yield in the enzymolysis liquid of second segment alkali alcohol pre-treatment residue,
Growth rate is respectively 18.2% and 8.2%.
Compared with Example 2, the glucose yield of embodiment 2 is slightly higher, and the cellulase dosage of embodiment 2 for comparative example 1
The only half of comparative example 1, this illustrates that the addition of Tween 80 can save half in the case where keeping the comparable situation of glucose yield
Cellulase dosage.
Comparative example 2
Comparative example 2 is similar to Example 2, and difference is, takes 5 grams of (in terms of over dry) first segment dilute sulfuric acid pretreatments respectively
Residue and second segment alkali alcohol pre-treatment residue are separately added into the pH=in cellulase (match two generation of power) and 250mL of 100FPU
4.8 acetic acid-sodium acetate buffer solution is digested.Controlled at 50 DEG C in reaction process, revolving speed is 150 revs/min.Enzymatic hydrolysis
10min inactivation treatment is taken out and carried out after carrying out 72 hours, using the method separation enzymolysis liquid and enzymatic hydrolysis residue of vacuum filtration, is used
Efficient liquid phase measures concentration of glucose in enzymolysis liquid, and calculating gained glucose yield is respectively 63.2% and 61.6%.
Other raw material dosages and operating procedure are same as Example 2.
Comparative example 2 compared with Example 3, in the comparable situation of glucose yield, the addition of Tween 80 in enzymolysis process
Enzymolysis time be can be shortened to 24 hours.Enzymatic hydrolysis condition is identical, when enzymolysis time is 72 hours, Tween 80 is added and does not add tween
80 first segment high-temperature-hot-water pretreatment residue is compared with glucose yield in the enzymolysis liquid of second segment alkali alcohol pre-treatment residue,
Growth rate is respectively 12.2% and 23.4%.
Compared with Example 4, the glucose yield of embodiment 4 is slightly higher, and the cellulase dosage of embodiment 4 for comparative example 2
The only half of comparative example 2, this illustrates that the addition of Tween 80 can save half in the case where keeping the comparable situation of glucose yield
Cellulase dosage.
It by the comparison of comparative example and corresponding embodiment, can learn in the comparable situation of glucose yield, digest
The addition of Tween 80 can greatly shorten enzymolysis time in the process；When enzymatic hydrolysis condition is identical with enzymolysis time, spat in enzymolysis process
The addition of temperature 80 can greatly improve the yield of glucose；Enzymolysis time is identical, when enzymatic hydrolysis glucose yield is suitable, digests
The addition of Tween 80 can be greatly saved the dosage of cellulase in journey.The addition of Tween 80 can in enzymolysis process known to and then
Enzymolysis efficiency is greatly improved.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (9)
1. a kind of method for improving Heating Explosion Sugarcane Bagasse efficiency by two stages pretreatment and additive, which is characterized in that including following step
It is rapid:
S1. Bagasse Material and a certain amount of distilled water or 1% sulfuric acid solution are placed in closed reactor, at 100~130 DEG C
It reacts 20~40min and carries out first segment pretreatment, separate to obtain first segment pretreatment residue；
S2. a certain amount of first segment pretreatment residue and a certain amount of alkali ethyl alcohol are placed in closed reactor, 100~130
40~80min is reacted at DEG C and carries out second segment pretreatment, separates to obtain second segment pretreatment residue；
S3. the resulting pretreatment residue of a certain amount of step S1 and step S2 is taken respectively, and acetic acid-acetate buffer is added to it
Liquid, cellulase and additive, are digested, inactivation, and are measured to concentration of glucose.
2. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, in the step S1, the Bagasse Material is part remaining after squeezing sugar from the sugarcane that sugar refinery obtains, through air-drying
It crushes and obtains afterwards.
3. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
Be characterized in that, in the step S1, the mass volume ratio of the Bagasse Material and distilled water or 1% sulfuric acid solution be 1:8~
15。
4. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, in the step S2, alkali concentration is 0.3~0.6% in the alkali ethanol pre-treatment process, ethanol/water solution body
Product is than being 50/50~70/30.
5. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, it is described to be separated into vacuum filtration or centrifugation in the step S1 and step S2.
6. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
Be characterized in that, in the step S3, the enzyme digestion reaction time be 6~72 hours, temperature be 45~55 DEG C, revolving speed be 100~
200 revs/min, the pH of buffer is 4.5~6.0, and the dosage of cellulase and additive is relative to residue over dry matter after pretreatment
Amount is respectively 10~20FPU/ grams and 100~200 milligrams per grams.
7. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, in the step S3, the inactivation treatment for carrying out 5~15min to it is needed after the completion of the enzymolysis process.
8. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, in the step S3, the measuring method for carrying out glucose concentration determination is high-efficient liquid phase technique.
9. a kind of method that Heating Explosion Sugarcane Bagasse efficiency is improved by two stages pretreatment and additive according to claim 1,
It is characterized in that, in the step S3, the additive is Tween 80.
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| CN113122587A (en) * | 2021-06-04 | 2021-07-16 | 华南农业大学 | Method for promoting poplar to produce ethanol by hydrothermal combination with NaOH aqueous solution pretreatment |
| CN113914125A (en) * | 2021-10-18 | 2022-01-11 | 华南农业大学 | Method for separating cellulose from bagasse and carrying out enzymolysis |
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| CN113122587A (en) * | 2021-06-04 | 2021-07-16 | 华南农业大学 | Method for promoting poplar to produce ethanol by hydrothermal combination with NaOH aqueous solution pretreatment |
| CN113122587B (en) * | 2021-06-04 | 2022-07-08 | 华南农业大学 | Method for promoting poplar to produce ethanol by hydrothermal combination with NaOH aqueous solution pretreatment |
| CN113914125A (en) * | 2021-10-18 | 2022-01-11 | 华南农业大学 | Method for separating cellulose from bagasse and carrying out enzymolysis |
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