CN104231098A - Method for preparing xylooligosaccharide from bagasse by ethanol/water pretreatment - Google Patents
Method for preparing xylooligosaccharide from bagasse by ethanol/water pretreatment Download PDFInfo
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Abstract
The invention provides a method for preparing xylooligosaccharide from bagasse by ethanol/water pretreatment. The method comprises the following steps: mixing dried and pulverized bagasse raw material with an ethanol/water solution, obtaining a xylooligosaccharide solution with different yields by controlling the reaction temperature, reaction time, ethanol concentration and acetic acid consumption, carrying out ion exchange resin column chromatography on the xylooligosaccharide solution to remove impurities, and carrying out freeze drying or spray drying to obtain the xylooligosaccharide with higher purity. The pretreatment residue can be subjected to enzymolysis and fermentation to prepare energies and chemical products with high added value. Compared with the xylooligosaccharide prepared by the traditional biological enzyme process, the method has the advantages of simple technique, low cost and shorter production cycle, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method of biomass efficient Conversion with the use, particularly a kind of is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse.
Background technology
Xylo-oligosaccharide, also known as wood oligose, is a kind of naturally occurring functional polymerization sugar, is combined into by 2-7 wood sugar molecule with β-Isosorbide-5-Nitrae glycosidic link.Xylo-oligosaccharide is soluble in water, viscosity is lower, low-heat low energy, sugariness is equivalent to 40% of sucrose, effectively can prevent dental decayed tooth, promote calcium absorption, suppress physico-chemical property and the physiological function such as enteric pathogenic bacteria, as one safely and effectively additive can be widely used in the fields such as food, healthcare products, medicine, feed and agricultural.
Xylo-oligosaccharide exists with free and polymerization two kinds of forms at occurring in nature.Free xylo-oligosaccharide is present in fruit, vegetables and honey, but content is all considerably less.In most cases, xylo-oligosaccharide is present in the hemicellulose of plant with the form of xylan, coexists with Mierocrystalline cellulose, xylogen.Bagasse is as the principal by product of sugar industry, it is a kind of important renewable biomass resource, due to its source concentrate, output is large and be rich in hemicellulose, can meet the production of xylo-oligosaccharide, therefore bagasse is the high quality raw material being prepared xylo-oligosaccharide by lignocellulose raw material.
The method of production xylo-oligosaccharide conventional at present obtains for passing through xylanase hydrolysis hemicellulose, the shortcomings such as it is long that it exists the production cycle, and production cost is high.Seek from the hemicellulose of plant fiber material, prepare the method extracting xylo-oligosaccharide how efficiently very urgent.The present invention proposes a kind of is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, effectively can improve the production efficiency of xylo-oligosaccharide, reduce its production cost, and after pre-treatment, the solid residue of gained can pass through enzymolysis, fermentation for the chemicals of the energy and high added value.
Summary of the invention
The invention provides a kind of is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, and its alternative enzymolysis produces xylo-oligosaccharide, simplifies production technique, enhances productivity, realize the recycling to lignocellulose raw material.
For achieving the above object, the technical solution used in the present invention is:
Be that raw material prepares a method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, comprise the following steps:
(1) Bagasse Material and aqueous ethanolic solution are placed in closed reactor, at 160 ~ 200 DEG C, under acetic acid effect, react 30 ~ 90min, be separated, obtain pretreatment fluid and pre-treatment residue; Described acetic acid add-on is equivalent to 0 ~ 10wt% of the quality of Bagasse Material;
(2) add deionized water precipitation lignin in the pretreatment fluid of step (1) gained, be separated, obtain the solution being rich in xylo-oligosaccharide;
(3) step (2) gained is rich in the solution of xylo-oligosaccharide through ion exchange resin column chromatography removal impurity wherein, obtains solution;
(4) solution of step (3) gained obtains xylo-oligosaccharide through lyophilize or spraying dry.
In aforesaid method, Bagasse Material described in step (1) is part remaining after the sugarcane obtained from sugar refinery squeezes sugar, and thread rolling after air-dry, pulverizing obtain.
In aforesaid method, described in step (1), the weightmeasurement ratio of Bagasse Material and ethanol/water solution is 1:5 ~ 10g/mL; In described aqueous ethanolic solution, the volume ratio of ethanol and water is 40/60 ~ 80/20.
In aforesaid method, described in step (1), be separated into filtration, filter press or centrifugal.
In aforesaid method, the consumption of step (2) described deionized water is 1 ~ 3 times of pretreatment fluid volume.
In aforesaid method, described in step (2), be separated into filtration, filter press or centrifugal.
In aforesaid method, the described removal impurity of step (3) comprises formic acid, acetic acid, furfural and glucuronic acid.
Aforesaid method achieves prepares xylo-oligosaccharide through ethanol/water through pre-treatment by Bagasse Material.
Compared with prior art, the advantage that has of the present invention and effect as follows:
1, the present invention's alternative Traditional Wood glycan enzyme-squash techniqued xylo-oligosaccharide, reduces production cost, shortens and produces
Cycle.
2, the xylo-oligosaccharide yield that the present invention can be higher.
3, the present invention's ethanol used through distillation reuse, can reduce chemical consumption and environmental pollution.
4, remaining solid residue rich cellulose composition of the present invention, can be used for papermaking or fermentation for the energy and height
The chemicals of added value.
Embodiment
Do specifically to describe in detail further to the present invention below in conjunction with specific embodiment, but embodiments of the present invention are not limited thereto, for the processing parameter do not indicated especially, can refer to routine techniques and carry out.
Bagasse Material used takes from sugar refinery, its particle diameter <1 millimeter after air-dry, thread rolling, pulverization process, and its component is dextran 39.35%, xylan 21.64%, arabinan 1.64%, Polygalactan 0.37%, acid insoluble lignin 24.31%, ash content 4.51%.
Wood sugar and xylo-oligosaccharide content ion chromatography analysis in pretreatment fluid, the method for calculation of its wood sugar or xylo-oligosaccharide are as follows:
In formula, Y represents wood sugar or xylo-oligosaccharide yield (gram/100 grams of raw materials); C represents the concentration (g/L) of wood sugar or xylo-oligosaccharide in pretreatment fluid; V represents the volume (L) of pretreatment fluid; M represents the quality (g) of Bagasse Material.
Embodiment 1
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 170 DEG C and start timing, the question response time is when reaching 60 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get pretreatment fluid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 2
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 60 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 3
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 45 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 4
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 90 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 5
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (40/60, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 45 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 6
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (80/20, v/v), and add 25 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 45 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 7
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), do not adding under acetic acid, opening stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 45 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.Then the pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Embodiment 8
Take 500 grams of over dry Bagasse Materials and be placed in the closed reactor that thermopair is housed, add 4000mL water/ethanolic soln (60/40, v/v), and add 50 grams of acetic acid, open stirring, heating system, make temperature rise to 190 DEG C and start timing, the question response time is when reaching 45 minutes, stop heating, and make reaction be down to room temperature with water of condensation immediately, adopt the method separation and culture liquid and pre-treatment residue that filter.
Get alcohol pre-treatment liquid 1000mL, add 2000mL deionized water, in order to precipitate lignin, and centrifugation lignin and pretreatment fluid, with Xylose Content in ion chromatography pretreatment fluid.The pretreatment fluid that 50mL dilutes is joined 250mL 3% (w/w) H
2sO
4in, and boil 4h, make xylo-oligosaccharide wherein be hydrolyzed into wood sugar, by its total wood sugar amount of ion chromatography.Xylo-oligosaccharide amount is total wood sugar amount and the difference of the wood sugar in the pretreatment fluid directly measured.Pretreatment section wood sugar and xylo-oligosaccharide yield are in table 1.
Alcohol pre-treatment liquid spent ion exchange resin column chromatography after lignin precipitation removes formic acid, acetic acid, furfural and glucuronic acid impurity wherein, obtains xylo-oligosaccharide through concentrated postlyophilization.
Table 1
Be 60min in the reaction times as can be seen from Table 1, ethanol/water volume ratio is 60/40 (v/v), under the effect of 5wt% acetic acid, when temperature rises to 190 DEG C by 170 DEG C, wood sugar yield (by 0.14 gram to 0.56 gram/100 grams raw materials) and xylo-oligosaccharide yield (by 6.07 grams to 11.27 grams/100 grams raw materials) raise all to some extent, now the transformation efficiency of xylo-oligosaccharide is maximum, is 45.83%.
It is 190 DEG C in temperature of reaction, ethanol/water volume ratio is 60/40, under the effect of 5wt% acetic acid, when the time rises to 60min by 45min, xylo-oligosaccharide yield is by 10.71 gram liters to 11.27 gram/100 grams of raw materials, and when the time extends to 90min, the yield of xylo-oligosaccharide is down to 8.42 grams/100 grams raw materials.
It is 190 DEG C in temperature of reaction, reaction times is 45min, under the effect of 5wt% acetic acid, when ethanol/water solution volume ratio 40/60 rises to 60/40, xylo-oligosaccharide yield is by 6.86 gram liters to 10.71 gram/100 grams of raw materials, and when ethanol/water solution volume ratio 80/20, xylo-oligosaccharide yield is only 2.92 grams/100 grams raw materials.
It is 190 DEG C in temperature of reaction, reaction times is 45min, when ethanol/water volume ratio is 60/40, with the reacting phase ratio not having acetic acid effect, under the effect of 5wt% acetic acid, the yield of xylo-oligosaccharide has a distinct increment, by 7.13 gram liters to 10.71 gram/100 grams of raw materials, when continuation improves acetic acid consumption (10wt%), the yield of xylo-oligosaccharide does not have sustainable growth, decrease to some degree on the contrary (7.31 grams/100 grams raw materials).
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 exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (7)
1. be that raw material prepares a method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, it is characterized in that, comprise the following steps:
(1) Bagasse Material and aqueous ethanolic solution are placed in closed reactor, at 160 ~ 200 DEG C, under acetic acid effect, react 30 ~ 90 min, be separated, obtain pretreatment fluid and pre-treatment residue; Described acetic acid add-on is equivalent to 0 ~ 10 wt% of the quality of Bagasse Material;
(2) add deionized water precipitation lignin in the pretreatment fluid of step (1) gained, be separated, obtain the solution being rich in xylo-oligosaccharide;
(3) step (2) gained is rich in the solution of xylo-oligosaccharide through ion exchange resin column chromatography removal impurity wherein, obtains solution;
(4) solution of step (3) gained obtains xylo-oligosaccharide through lyophilize or spraying dry.
2. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, it is characterized in that, Bagasse Material described in step (1) is part remaining after the sugarcane obtained from sugar refinery squeezes sugar, and thread rolling after air-dry, pulverizing obtain.
3. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, and it is characterized in that, described in step (1), the weightmeasurement ratio of Bagasse Material and ethanol/water solution is 1:5 ~ 10 g/mL; In described aqueous ethanolic solution, the volume ratio of ethanol and water is 40/60 ~ 80/20.
4. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, it is characterized in that, is separated into filtration, filter press or centrifugal described in step (1).
5. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, and it is characterized in that, the consumption of step (2) described deionized water is 1 ~ 3 times of pretreatment fluid volume.
6. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, it is characterized in that, is separated into filtration, filter press or centrifugal described in step (2).
7. according to claim 1 is that raw material prepares the method for xylo-oligosaccharide through ethanol/water pre-treatment with bagasse, and it is characterized in that, the described removal impurity of step (3) comprises formic acid, acetic acid, furfural and glucuronic acid.
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| CN108486285A (en) * | 2018-02-09 | 2018-09-04 | 北京林业大学 | A kind of method of acetyl group auxiliary xylooligosaccharides production |
| CN109825542A (en) * | 2019-03-04 | 2019-05-31 | 齐鲁工业大学 | A method of it removing lignin in hot water pre-hydrolyzed solution and prepares xylo-oligosaccharide |
| CN111100216A (en) * | 2019-12-19 | 2020-05-05 | 上海昶法新材料有限公司 | Process method for co-producing oligosaccharide, lignin and unbleached pulp by using branch wood plant waste as raw material |
| CN111100305A (en) * | 2019-12-30 | 2020-05-05 | 上海昶法新材料有限公司 | Process method for co-producing oligosaccharide, lignin and unbleached pulp by taking residues of alcohol production through corn straw fermentation as raw materials |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108486285A (en) * | 2018-02-09 | 2018-09-04 | 北京林业大学 | A kind of method of acetyl group auxiliary xylooligosaccharides production |
| CN109825542A (en) * | 2019-03-04 | 2019-05-31 | 齐鲁工业大学 | A method of it removing lignin in hot water pre-hydrolyzed solution and prepares xylo-oligosaccharide |
| CN111100216A (en) * | 2019-12-19 | 2020-05-05 | 上海昶法新材料有限公司 | Process method for co-producing oligosaccharide, lignin and unbleached pulp by using branch wood plant waste as raw material |
| CN111100305A (en) * | 2019-12-30 | 2020-05-05 | 上海昶法新材料有限公司 | Process method for co-producing oligosaccharide, lignin and unbleached pulp by taking residues of alcohol production through corn straw fermentation as raw materials |
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