CN101624610A - Method for efficiently saccharifying xylose residue - Google Patents
Method for efficiently saccharifying xylose residue Download PDFInfo
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- CN101624610A CN101624610A CN200910090186A CN200910090186A CN101624610A CN 101624610 A CN101624610 A CN 101624610A CN 200910090186 A CN200910090186 A CN 200910090186A CN 200910090186 A CN200910090186 A CN 200910090186A CN 101624610 A CN101624610 A CN 101624610A
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Abstract
The invention relates to a method for efficiently saccharifying xylose residue. The method comprises the following steps: mixing xylose residues and catalyst aqueous solution with the concentration in percentage by mass of 1 percent-20 percent; heating the mixture to react at 70 DEG C-180 DEG C for 10 minutes to 400 minutes; and after solid and liquid are separated, carrying out enzymolysis on the obtained solid, wherein the catalyst is a mixture of sodium hydroxide solution and sodium sulfite solution. Sugar liquor obtained by enzymolysis according to the method has high concentration, the total sugar content can reach more than 15 percent, and the defect of low concentration of other lignocellulose enzymolysis sugar liquors is overcome; the enzymolysis liquor has high glucose purity and less residual sugar content, and the sugar liquor can meet the requirement of other fermentation technologies; the lignin content of stewed black liquor and the quality of sulfonated lignin are high, and the problem of stewing black liquor wastewater by an alkaline method is solved.
Description
Technical field
The present invention relates to technical field of biochemical industry, be specifically related to a kind of method the xylose residue efficiently saccharifying.
Background technology
Estimating as the petroleum resources of world economy pillar will be exhausted about many decades, and therefore, the development research of oil substitutes is extremely urgent.It is that raw material prepares alcohol fuel with biotransformation method in research with wooden Biological resources that a lot of countries are arranged at present, to substitute or the alternative limited oil of reserves of part.
The main component of wooden Biological resources is Mierocrystalline cellulose, hemicellulose and lignin.Wherein, Mierocrystalline cellulose, hemicellulose are the sources of fermentable sugars, and content accounts for 66～75 (oven dry weights of cellulose raw material).Generating ethanol by hexose by fermentation by saccharomyces cerevisiae is very sophisticated technology, when adopting the wooden Biological resources of cellulase hydrolysis to make ethanol, cellulase must contact to be adsorbed onto reaction is carried out, therefore, Mierocrystalline cellulose is the key factor of decision hydrolysis rate to the accessibility of cellulase.
The principal element that influences cellulase hydrolysis has the content of lignin in the Mierocrystalline cellulose, cellulosic specific surface area and the cellulosic degree of crystallinity and the polymerization degree, studies show that, xylogen has played certain shielding effect when enzymolysis, content of lignin is big more, and enzymatic hydrolyzation is low more; Therefore lignocellulose-like biomass improves enzymatic hydrolyzation as if wanting, should reduce the xylogen amount in the Mierocrystalline cellulose, and the hemicellulose amount that reduces wherein reduces the cellulosic degree of crystallinity and the polymerization degree simultaneously, the plain and enzyme contacted specific surface area with increased fiber;
Summary of the invention
The purpose of this invention is to provide a kind of method, to solve the prior art above shortcomings with the xylose residue efficiently saccharifying.
The invention provides a kind of method with the xylose residue efficiently saccharifying, comprise xylose residue and concentration being that the aqueous catalyst solution of 1～20% (wt/wt) mixes, be heated to 70 ℃～180 ℃ and reacted 10～400 minutes down, after the solid-liquid separation, the solid that obtains is carried out enzymolysis; Described catalyzer is sodium hydroxide solution and sodium sulfite aqueous solution mixture.
Wherein, the weightmeasurement ratio of described xylose residue oven dry weight and aqueous catalyst solution is 1: 1～20; Described xylose residue is selected from residue after furfural dregs, the corn cob acid hydrolysis or the residue after the bagasse hydrolysis.
Preferably, the weightmeasurement ratio of described xylose residue oven dry weight and aqueous catalyst solution is 1: 4～10.
The mass percent concentration of described sodium hydroxide solution is 1～10%, and the mass percent concentration of sodium sulfite solution is 0.1～20%.
After the solid-liquid separation, wash solid product with water, solid is dropped in the reactor by certain concentration, regulate pH and temperature, add corresponding enzyme and carry out enzymolysis, obtain glucose, then by other biochemical industry product of glucose fermentation; The present invention uses cellulase to carry out enzymolysis, and its add-on is 10～30FPIU/ gram substrate, and the pH value is 4.5～5.2, and temperature is at 46～50 ℃, and enzymolysis time is 48～72 hours.
The liquid phase that obtains after the solid-liquid separation (black digestion liquid) behind membrane concentration, further concentrates and makes the sulfonated lignin product, has reduced pretreated cost.
The present invention has following beneficial effect with the method for xylose residue efficiently saccharifying:
1) the sugar concentration height that obtains of enzymolysis, total reducing sugar can reach more than 15%, has overcome the low shortcoming of other lignocellulose enzymolysis sugar concentration;
2) enzymolysis solution glucose purity height, assorted sugared content is less, and liquid glucose can satisfy the requirement of other zymotechnique;
3) lignin content height in the black digestion liquid, the sulfonated lignin quality that obtains is good, has solved the difficult problem of alkaline cooking black liquor waste.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Used cellulase is the plain enzyme of commercial fibre that Wuxi biotechnology company limited of outstanding energy section produces among the following embodiment.
Embodiment 1
In a suitable reactor, residue after the corn cob acid hydrolysis of adding 4000 gram water content 70%, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (the residue oven dry weight after the corn cob acid hydrolysis and the weight ratio of aqueous catalyst solution), sodium hydroxide lye concentration 2.0%, concentration of sodium sulfite is 1%, after sealing mouth, pre-treatment was carried out in heating in 1.5 hours under 85 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 62.4% after the pre-treatment, total sugar concentration 16.2%, glucose purity 90.5%, cellulase hydrolysis yield 88.5%.
Embodiment 2
In a suitable reactor, residue after the corn cob acid hydrolysis of adding 4000 gram water content 70%, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (weight ratio of corn cob acid hydrolysis slag oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, the concentration of S-WAT is 0.8%, after sealing mouth, pre-treatment was carried out in heating in 1 hour under 95 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 63.4% after the pre-treatment, total sugar concentration 15.4%, glucose purity 91.5%, cellulase hydrolysis yield 87.6%.
Embodiment 3
In a suitable reactor, residue after the corn cob acid hydrolysis of adding 4000 gram water content 70%, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (weight ratio of corn cob acid hydrolysis slag oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, sulphidity is 1.5%, after sealing mouth, pre-treatment was carried out in heating in 1 hour under 95 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 62.8% after the pre-treatment, total sugar concentration 15.8%, glucose purity 92.4%, cellulase hydrolysis yield 88.4%.
Embodiment 4
In a suitable reactor, residue after the corn cob acid hydrolysis of adding 4000 gram water content 70%, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (weight ratio of corn cob acid hydrolysis slag oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, the concentration of S-WAT be 1.0% seal mouth after, pre-treatment was carried out in heating in 30 minutes under 170 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 50% after the pre-treatment, total sugar concentration 16.4%, glucose purity 96%, cellulase hydrolysis yield 90.6%.
Embodiment 5
In a suitable reactor, add the air-dry maize straw after 1200 grams shred, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 4 (weight ratio of maize straw oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, the concentration of S-WAT is 1.2%, after sealing mouth, pre-treatment was carried out in heating in 0.5 hour under 140 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 52.6% after the pre-treatment, enzymolysis total sugar concentration 12.2%, glucose purity 75.0%, enzymolysis total reducing sugars yield 85.5%.
Embodiment 6
In a suitable reactor, add the air-dry maize straw after 1200 grams shred, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (weight ratio of maize straw oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, the concentration of S-WAT is 1.2%, after sealing mouth, pre-treatment was carried out in heating in 1.5 hours under 85 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 63.6% after the pre-treatment, enzymolysis total sugar concentration 10.2%, glucose purity 74.6%, enzymolysis total reducing sugars yield 83.5%.
Embodiment 7
In a suitable reactor, the air-dry sucrose slag that adds 2000 grams, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 7 (weight ratio of bagasse oven dry weight and aqueous catalyst solution), concentration of lye 2.0%, the concentration of S-WAT is 1.0%, seal mouth after, pre-treatment was carried out in heating in 1.0 hours under 95 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, and the black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 62.3% after the pre-treatment, enzymolysis total sugar concentration 12.8/%, glucose purity 80.2%, enzymolysis total reducing sugars yield 86.5%.
Embodiment 8
In a suitable reactor, the air-dry sucrose slag that adds 2000 grams, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 10 (weight ratio of bagasse oven dry weight and aqueous catalyst solution), concentration of lye 1.0%, the concentration of S-WAT is 18%, seal mouth after, pre-treatment was carried out in heating in 1.0 hours under 105 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, and the black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.8, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 60.8% after the pre-treatment, enzymolysis total sugar concentration 13.4/%, glucose purity 79.5%, enzymolysis total reducing sugars yield 87.5%.
Embodiment 9
In a suitable reactor, slag after the corn cob acid hydrolysis of adding 4000 gram water content 70%, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 1 (weightmeasurement ratio of slag oven dry weight and aqueous catalyst solution after the corn cob acid hydrolysis), concentration of lye 10%, the concentration of S-WAT is 10%, after sealing mouth, pre-treatment was carried out in heating in 6 hours under 70 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 4.5, attemperation to 50 ℃ adds cellulase in feed liquid, with the enzyme amount is 30FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 48 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 62.4% after the pre-treatment, glucose purity 85.9%, total sugar concentration 14.2%, cellulase hydrolysis yield 88.5%.
Embodiment 10
In a suitable reactor, add the air-dry maize straw after 1200 grams shred, the sodium hydroxide and the S-WAT mixing solutions that add heat then in the ratio of solid-to-liquid ratio 1: 20 (weight ratio of maize straw oven dry weight and aqueous catalyst solution), concentration of lye 1.5%, the concentration of S-WAT is 0.5%, after sealing mouth, pre-treatment was carried out in heating in 10 minutes under 180 ℃ of conditions, the slurries that obtain are centrifugal in the 2000rpm whizzer, black liquor after centrifugal is made the sulfonated lignin product after evaporation concentration; The gained solid phase adds in the reactor, add a certain amount of water simultaneously, with acid for adjusting pH to 5.2, attemperation to 46 ℃ adds cellulase in feed liquid, with the enzyme amount is 10FPIU/ gram substrate (in butt), mixing speed 100rpm/min, enzymolysis time were controlled at 72 hours, and sampling in per 24 hours once, utilize the DNS method survey enzymolysis solution total sugar concentration, utilize high performance liquid chromatography to survey total reducing sugars concentration in the enzymolysis solution; Obtain that the solid yield is 48.6% after the pre-treatment, enzymolysis total sugar concentration 10.2%, glucose purity 78.2%, enzymolysis total reducing sugars yield 83.5%.
Claims (6)
1, a kind of method with the xylose residue efficiently saccharifying, it is characterized in that it is that 1～20% aqueous catalyst solution mixes that this method comprises xylose residue and mass percent concentration, be heated to 70 ℃～180 ℃ reactions 10～400 minutes down, after the solid-liquid separation, the solid that obtains is carried out enzymolysis; Described catalyzer is the mixture of sodium hydroxide solution and sodium sulfite solution.
According to the described method of claim 1, it is characterized in that 2, described xylose residue is selected from residue after furfural dregs, the corn cob acid hydrolysis or the residue after the bagasse hydrolysis with the xylose residue efficiently saccharifying.
According to the described method with the xylose residue efficiently saccharifying of claim 1, it is characterized in that 3, the mass percent concentration of described sodium hydroxide solution is 1～10%, the mass percent concentration of sulfurous acid solution is 0.1～20%.
According to the described method of claim 1, it is characterized in that 4, the weight ratio of described xylose residue oven dry weight and aqueous catalyst solution is 1: 1～20 with the xylose residue efficiently saccharifying.
According to the described method of claim 4, it is characterized in that 5, the weight ratio of described xylose residue oven dry weight and aqueous catalyst solution is 1: 4～10 with the xylose residue efficiently saccharifying.
6, according to the described method with the xylose residue efficiently saccharifying of claim 1, it is characterized in that, use cellulase to carry out enzymolysis, its add-on is 10～30FPIU/ gram substrate, and the pH value is 4.5～5.2, and temperature is at 46～50 ℃, and enzymolysis time is 48～72 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102816813A (en) * | 2012-09-10 | 2012-12-12 | 北京林业大学 | Method for pretreating and efficiently saccharifying furfural residues |
| CN104520446A (en) * | 2012-08-10 | 2015-04-15 | 东丽株式会社 | Method for producing sugar solution |
| CN106978448A (en) * | 2017-03-22 | 2017-07-25 | 中溶科技股份有限公司 | A kind of method and system of xylose residue efficient anaerobic producing methane |
-
2009
- 2009-07-31 CN CN200910090186A patent/CN101624610A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104520446A (en) * | 2012-08-10 | 2015-04-15 | 东丽株式会社 | Method for producing sugar solution |
| CN104520446B (en) * | 2012-08-10 | 2016-10-05 | 东丽株式会社 | The manufacture method of sugar liquid |
| US9951393B2 (en) | 2012-08-10 | 2018-04-24 | Toray Industries, Inc. | Method of producing sugar solution |
| CN102816813A (en) * | 2012-09-10 | 2012-12-12 | 北京林业大学 | Method for pretreating and efficiently saccharifying furfural residues |
| CN106978448A (en) * | 2017-03-22 | 2017-07-25 | 中溶科技股份有限公司 | A kind of method and system of xylose residue efficient anaerobic producing methane |
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Application publication date: 20100113 |