CN104073532A - Method for preparing xylose and glucose by pre-treating bagasse materials - Google Patents
Method for preparing xylose and glucose by pre-treating bagasse materials Download PDFInfo
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- CN104073532A CN104073532A CN201410252922.1A CN201410252922A CN104073532A CN 104073532 A CN104073532 A CN 104073532A CN 201410252922 A CN201410252922 A CN 201410252922A CN 104073532 A CN104073532 A CN 104073532A
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Abstract
The invention provides a method for preparing xylose and glucose by pre-treating bagasse materials. The method comprises the following steps of: (1) placing bagasse materials and water into a sealed reactor, introducing 1-7 MPa CO2, reacting for 20-100 minutes at 140-180 DEG C, separating to obtain pre-treated liquor and pre-treated residues; (2) adding buffer liquor and compound cellulose into the pre-treated residues obtained in the step (1), carrying out enzymolysis, inactivating and separating to obtain enzymatic hydrolysate and enzymolysis residues; and (3), combining pretreated liquor obtained in the step (1) with enzymatic hydrolysate obtained in the step (2) to obtain liquor rich in xylose and glucose. The method disclosed by the invention adopts an environment-friendly type pretreatment method to carry out pretreatment and enzymolysis saccharification on bagasse materials; by analyzing components of the pretreated liquor and enzymatic hydrolysate, the yield of xylose and glucose is known to be higher, and therefore, the method has good application prospect.
Description
Technical field
The present invention relates to a kind of method of preparing xylose and glucose, particularly a kind of method of being prepared xylose and glucose by Bagasse Material through pre-treatment.
Background technology
Along with the continuous of the problem such as shortage and environment of the energy given prominence to, biomass, as the renewable resources that can be converted into liquid fuel, come into one's own just day by day.In abundant biomass resource, paid close attention to by people with wooden fine fiber biomass prepare liquid fuel on earth.
The method of wood fiber biomass prepare liquid fuel is that the hemicellulose in this raw material, cellulose hydrolysis are become to the monose such as wood sugar, glucose, by aqueous catalysis condensation, dehydration-hydrogenation-isoparaffin synthetic fluid fuel.Prepare by wood fiber biomass raw material the prerequisite that the monose such as wood sugar, glucose is its prepare liquid fuel.But because the Mierocrystalline cellulose in raw material and hemicellulose and lignin closely link together, make its stable in properties, be difficult for being destroyed by cellulase, therefore need biomass material to carry out pre-treatment.Pre-treatment can Partial digestion hemicellulose and/or lignin, breaks the reticulated structure that hemicellulose and lignin form, and Mierocrystalline cellulose is separated with lignin with hemicellulose, improves the porosity of matrix, to improving its enzymolysis accessibility, and then improves enzymolysis efficiency.
Bagasse is as the main byproduct of sugar industry, it is a kind of important renewable biomass resource, because concentrate in its source, output is large and rich cellulose, hemicellulose, can meet the production of high value added product, therefore bagasse is the high quality raw material of being prepared wood sugar, glucose by wood fiber biomass raw material.Conventional pretreatment process has acid system pre-treatment, alkaline process pre-treatment, organic solvent pre-treatment and ionic liquid pretreatment etc. at present.Although their extracting parts effectively hemicellulose and/or lignin, and then improve follow-up cellulosic enzyme digestion reaction, its production cost is high, contaminated wastewater environment.Find a kind of cheapness, environmentally friendly pretreatment process very urgent.
Summary of the invention
The invention provides a kind of method of being prepared xylose and glucose by Bagasse Material through pre-treatment, its alternative acid, alkali, organic solvent and ionic liquid, improve the transformation efficiency that the biomass materials such as bagasse are prepared xylose and glucose.
For achieving the above object, the technical solution used in the present invention is:
(1) Bagasse Material and water are placed in to closed reactor, pass into 1～7MPa CO
2, at 140～180 DEG C, react 20～100min, separate, obtain pretreatment fluid and pre-treatment residue;
(2) in the pre-treatment residue of step (1) gained, add damping fluid and complex cellulase, carry out enzymolysis, deactivation, separates, and obtains enzymolysis solution and enzymolysis residue;
(3) pretreatment fluid of gained and the enzymolysis solution of step (2) gained in step (1), be the solution that is rich in xylose and glucose product.
In aforesaid method, Bagasse Material described in step (1) is remaining part the sugarcane squeezing sugar of obtaining from sugar refinery, and thread rolling after air-dry, pulverizing obtain.
In aforesaid method, described in step (1), the mass ratio of Bagasse Material and water is 1:5～10.
In aforesaid method, step is separated into vacuum filtration or centrifugal described in (1).
In aforesaid method, the described enzyme digestion reaction time of step (2) is 48～72 hours, and temperature is 45～55 DEG C, and rotating speed is 100～200 revs/min, the pH of damping fluid is 4.5～6.0, complex cellulase with respect to pre-treatment after the consumption of residue over dry quality be 10～20FPU/ gram.
In aforesaid method, the described damping fluid of step (2) is acetic acid-sodium acetate buffer.
In aforesaid method, after completing, the described enzymolysis process of step (2) needs it to carry out the inactivation treatment of 5～15min.
In aforesaid method, step is separated into vacuum filtration or centrifugal described in (2).
Compared with prior art, the present invention has advantage and effect are as follows:
The pretreatment processs such as 1, the alternative traditional acid of the present invention, alkali, organic solvent, pre-treatment residue carries out follow-up enzymolysis not to be needed through washing, noresidue pollutent.
2, the present invention can carry out pre-treatment under compared with high solid-liquid ratio condition.
3, the present invention can be higher wood sugar, glucose and total reducing sugar yield.
Embodiment
Below in conjunction with specific embodiment, the present invention is done specifically to describe in detail further, but embodiments of the present invention are not limited to this, for not dated especially processing parameter, can carry out with reference to routine techniques.
Bagasse Material used is taken from sugar refinery, its particle diameter <1 millimeter after air-dry, thread rolling, pulverization process, and its component is dextran 37.22%, xylan 24.60%, arabinan 1.54%, Polygalactan 0.55%, ash content 4.59%.
Wood sugar or glucose content ion chromatography analysis in pretreatment fluid, the method for calculation of its wood sugar or glucose are as follows:
Y in formula
enzymeexpression monose yield (gram/100 grams of raw materials); C
enzymerepresent the concentration (g/L) of monose in pretreatment fluid; V
enzymerepresent the volume (L) of pretreatment fluid; M
enzymerepresent the quality (g) of enzymolysis pre-treatment residue used; W represents pre-treatment residue yield (%).
Embodiment 1
Take 45 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 300 ml deionized water, open and stir, pass into CO
2gas makes its pressure reach 5MPa, and heating makes temperature rapidly increase to 160 DEG C and start timing, and the question response time, while reaching 60 minutes, stops heating, and makes reaction be down to room temperature with water of condensation immediately, discharges fast CO wherein
2gas, adopt the method for vacuum filtration to separate pretreatment fluid and pre-treatment residue, measure wood sugar, glucose content in pretreatment fluid with Ion Chromatographic Method, wherein wood sugar and glucose content account for 93.54% of pretreatment fluid total reducing sugar (comprising wood sugar, glucose, pectinose, semi-lactosi).
Get 4 grams of pre-treatment residues (being equivalent to oven-dry weight) and add the complex cellulase (Jie Nengke biotechnology company limited, A30173G190) of 60FPU and the acetic acid sodium acetate buffer solution of the pH=4.8 of 200mL.In reaction process, controlling temperature is 50 DEG C, and rotating speed is 150 revs/min.Enzymolysis carries out after 60 hours, taking out and carrying out 10min inactivation treatment, adopts the method for vacuum filtration to separate enzymolysis solution and enzymolysis residue, with wood sugar, glucose content in Ion Chromatographic Method mensuration enzymolysis solution.
In pretreatment fluid and enzymolysis solution, xylose and glucose yield is in table 1.
Embodiment 2
Take 45 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 300 ml deionized water, open and stir, pass into CO
2gas makes its pressure reach 5MPa, and heating makes temperature rapidly increase to 160 DEG C and start timing, and the question response time, while reaching 80 minutes, stops heating, and makes reaction be down to room temperature with water of condensation immediately, discharges fast CO wherein
2gas, adopt the method for vacuum filtration to separate pretreatment fluid and pre-treatment residue, measure wood sugar, glucose content in pretreatment fluid with Ion Chromatographic Method, wherein wood sugar and glucose content account for 94.46% of pretreatment fluid total reducing sugar (comprising wood sugar, glucose, pectinose, semi-lactosi).
Get 4 grams of pre-treatment residues (being equivalent to oven-dry weight) and add the complex cellulase (Jie Nengke biotechnology company limited, A30173G190) of 60FPU and the acetic acid sodium acetate buffer solution of the pH=4.8 of 200mL.In reaction process, controlling temperature is 50 DEG C, and rotating speed is 150 revs/min.Enzymolysis carries out after 60 hours, taking out and carrying out 10min inactivation treatment, adopts the method for vacuum filtration to separate enzymolysis solution and enzymolysis residue, with wood sugar, glucose content in Ion Chromatographic Method mensuration enzymolysis solution.
In pretreatment fluid and enzymolysis solution, xylose and glucose yield is in table 1.
Embodiment 3
Take 45 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 300 ml deionized water, open and stir, pass into CO
2gas makes its pressure reach 5MPa, and heating makes temperature rapidly increase to 180 DEG C and start timing, and the question response time, while reaching 100 minutes, stops heating, and makes reaction be down to room temperature with water of condensation immediately, discharges fast CO wherein
2gas, adopt the method for vacuum filtration to separate pretreatment fluid and pre-treatment residue, measure wood sugar, glucose content in pretreatment fluid with Ion Chromatographic Method, wherein wood sugar and glucose content account for 94.25% of pretreatment fluid total reducing sugar (comprising wood sugar, glucose, pectinose, semi-lactosi).
Get 4 grams of pre-treatment residues (being equivalent to oven-dry weight) and add the complex cellulase (Jie Nengke biotechnology company limited, A30173G190) of 60FPU and the acetic acid sodium acetate buffer solution of the pH=4.8 of 200mL.In reaction process, controlling temperature is 50 DEG C, and rotating speed is 150 revs/min.Enzymolysis carries out after 60 hours, taking out and carrying out 10min inactivation treatment, adopts the method for vacuum filtration to separate enzymolysis solution and enzymolysis residue, with wood sugar, glucose content in Ion Chromatographic Method mensuration enzymolysis solution.
In pretreatment fluid and enzymolysis solution, xylose and glucose yield is in table 1.
Embodiment 4
Take 45 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 300 ml deionized water, open and stir, pass into CO
2gas makes its pressure reach 5MPa, and heating makes temperature rapidly increase to 160 DEG C and start timing, and the question response time, while reaching 100 minutes, stops heating, and makes reaction be down to room temperature with water of condensation immediately, discharges fast CO wherein
2gas, adopt the method for vacuum filtration to separate pretreatment fluid and pre-treatment residue, measure wood sugar, glucose content in pretreatment fluid with Ion Chromatographic Method, wherein wood sugar and glucose content account for 95.00% of pretreatment fluid total reducing sugar (comprising wood sugar, glucose, pectinose, semi-lactosi).
Get 4 grams of pre-treatment residues (being equivalent to oven-dry weight) and add the complex cellulase (Jie Nengke biotechnology company limited, A30173G190) of 60FPU and the acetic acid sodium acetate buffer solution of the pH=4.8 of 200mL.In reaction process, controlling temperature is 50 DEG C, and rotating speed is 150 revs/min.Enzymolysis carries out after 60 hours, taking out and carrying out 10min inactivation treatment, adopts the method for vacuum filtration to separate enzymolysis solution and enzymolysis residue, with wood sugar, glucose content in Ion Chromatographic Method mensuration enzymolysis solution.
In pretreatment fluid and enzymolysis solution, wood sugar, glucose and total reducing sugar yield are in table 1.
Table 1
To be Bagasse Material do not pass into CO to control group under 160 DEG C and 60min
2the pre-treatment of Shi Jinhang, enzymatic hydrolysis condition is consistent with above-described embodiment.
Be 160 DEG C at pretreatment condition as can be seen from Table 1, when 60min, do not pass into CO
2time total reducing sugar (xylose and glucose) yield be 36.12 grams/100 grams raw materials; At identical pretreatment time and temperature, pass into 5MPa CO
2time total reducing sugar yield be 47.29 grams/100 grams raw materials, subcritical CO of the present invention is described
2pretreatment process can improve total reducing sugar yield greatly.
Pretreatment process of the present invention is 5MPa CO at pretreatment condition
2, 160 DEG C, under 80min, it is maximum that wood sugar yield (pretreatment section wood sugar+enzymolysis section wood sugar) reaches, and is 18.79 grams/100 grams raw materials, accounts for 67.23% of total wood sugar in raw material.Be 5MPa CO at pretreatment condition
2, 180 DEG C, under 100min, it is maximum that glucose yield (pretreatment section glucose+enzymolysis section glucose) reaches, and is 38.78 grams/100 grams raw materials, accounts for 93.78% of total glucose in raw material.Be 5MPa CO at pretreatment condition
2, 160 DEG C, 100min, under, it is maximum that total reducing sugar yield (pretreatment section total reducing sugar+enzymolysis section total reducing sugar) reaches, and is 52.95 grams/100 grams raw materials, accounts for 76.41% of total reducing sugar in raw material.
The above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.All any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in the protection domain of the claims in the present invention.
Claims (8)
1. a method of being prepared xylose and glucose by Bagasse Material through pre-treatment, is characterized in that, comprises the following steps:
(1) Bagasse Material and water are placed in to closed reactor, pass into 1～7MPa CO
2, at 140～180 DEG C, react 20～100min, separate, obtain pretreatment fluid and pre-treatment residue;
(2) in the pre-treatment residue of step (1) gained, add damping fluid and complex cellulase, carry out enzymolysis, deactivation, separates, and obtains enzymolysis solution and enzymolysis residue;
(3) pretreatment fluid of gained and the enzymolysis solution of step (2) gained in step (1), be the solution that is rich in xylose and glucose product.
2. method according to claim 1, is characterized in that, Bagasse Material described in step (1) is remaining part the sugarcane squeezing sugar of obtaining from sugar refinery, and thread rolling after air-dry, pulverizing obtain.
3. method according to claim 1, is characterized in that, described in step (1), the mass ratio of Bagasse Material and water is 1:5～10.
4. method according to claim 1, is characterized in that, step is separated into vacuum filtration or centrifugal described in (1).
5. method according to claim 1, it is characterized in that, the described enzyme digestion reaction time of step (2) is 48～72 hours, temperature is 45～55 DEG C, rotating speed is 100～200 revs/min, the pH of damping fluid is 4.5～6.0, complex cellulase with respect to pre-treatment after the consumption of residue over dry quality be 10～20FPU/ gram.
6. method according to claim 1, is characterized in that, the described damping fluid of step (2) is acetic acid-sodium acetate buffer.
7. method according to claim 1, is characterized in that, needs it to carry out the inactivation treatment of 5～15 min after the described enzymolysis process of step (2) completes.
8. method according to claim 1, is characterized in that, step is separated into vacuum filtration or centrifugal described in (2).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878129A (en) * | 2015-04-08 | 2015-09-02 | 广东中烟工业有限责任公司 | Method for preparing tobacco xylose treating fluid by separation from bagasse, product and application of product |
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565725A (en) * | 2009-06-02 | 2009-10-28 | 天津大学 | Maize straw pretreatment method |
| WO2012075963A1 (en) * | 2010-12-10 | 2012-06-14 | Novozymes A/S | Methods for producing a fermentation product from lignocellulose-containing material |
| CN103243136A (en) * | 2013-05-08 | 2013-08-14 | 天津大学 | Method for improving enzymolysis saccharification efficiency of lignocellulose |
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2014
- 2014-06-09 CN CN201410252922.1A patent/CN104073532A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565725A (en) * | 2009-06-02 | 2009-10-28 | 天津大学 | Maize straw pretreatment method |
| WO2012075963A1 (en) * | 2010-12-10 | 2012-06-14 | Novozymes A/S | Methods for producing a fermentation product from lignocellulose-containing material |
| CN103243136A (en) * | 2013-05-08 | 2013-08-14 | 天津大学 | Method for improving enzymolysis saccharification efficiency of lignocellulose |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878129A (en) * | 2015-04-08 | 2015-09-02 | 广东中烟工业有限责任公司 | Method for preparing tobacco xylose treating fluid by separation from bagasse, product and application of product |
| CN107475467A (en) * | 2017-09-14 | 2017-12-15 | 齐鲁工业大学 | A kind of highly effective extraction method of poplar xylose |
| CN107475467B (en) * | 2017-09-14 | 2020-12-22 | 齐鲁工业大学 | Efficient extraction method of poplar xylose |
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Application publication date: 20141001 |