CN102839229B - Method for increasing reducing sugar yield by coupling of membrane separation and lignocellulose acid hydrolysis - Google Patents
Method for increasing reducing sugar yield by coupling of membrane separation and lignocellulose acid hydrolysis Download PDFInfo
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- CN102839229B CN102839229B CN201210340480.7A CN201210340480A CN102839229B CN 102839229 B CN102839229 B CN 102839229B CN 201210340480 A CN201210340480 A CN 201210340480A CN 102839229 B CN102839229 B CN 102839229B
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Abstract
The invention relates to a method for increasing reducing sugar yield by coupling of membrane separation and lignocellulose acid hydrolysis. The method is characterized in that hydrolytic reaction and the membrane separation are coupled to realize timely separation of hydrolysate and avoid continuous degradation of the hydrolysate, so that the reducing sugar yield is increased, fermentation inhibitors are prevented from being generated effectively, and subsequent fermentation is facilitated. According to the method, ordinary filtration, micro filtration and ultrafiltration are combined for use organically, the pollution of the hydrolysate to an ultrafiltration membrane is reduced effectively; and as various filter membrane retention substances return to a reaction kettle for continuous hydrolysis, the substrate conversion efficiency and the purity of the hydrolysate are improved, and the reducing sugar yield is increased.
Description
Invention field
The invention belongs to biomass resource trans-utilization technical field, particularly relate to a kind of method of utilizing membrane sepn and lignocellulose acid hydrolysis coupling to improve reducing sugar yield.
Background technology
Because shortage and the price of petroleum-based energy skyrocket, and the becoming increasingly conspicuous of environmental pollution, biomass come into one's own just day by day as the reproducible resource of one.
Lignocellulose three major polymers: cellulose, hemicellulose and three kinds, xylogen become to be grouped into.Wherein lignocellulose is the cellulose macromolecule being formed by connecting by β-Isosorbide-5-Nitrae glycosidic link by D-Glucose, and different cellulose macromolecules forms large polymer by hydrogen bond again, and its hydrolysate is glucose.Hemicellulose is the mixture being made up of different saccharans, and its hydrolysate is mainly wood sugar, pectinose and a small amount of hexose.Xylogen is the superpolymer with tridimensional network that a class is connected with C-C by ehter bond by phenylpropyl alcohol alkane unit, and it is formation protective layer around Mierocrystalline cellulose and hemicellulose, affects the hydrolysis of Mierocrystalline cellulose and hemicellulose.In lignocellulose resources development and utilization process, hydrolysis is one of committed step, and the main method for hydrolysis using is chemical hydrolysis and biological hydrolysis process in the world at present.
Wherein biological hydrolysis process mainly refers to enzymic hydrolysis.United States Patent (USP) 4,321,328 (Hoge) disclose a kind of technique of expecting ethanol from fiber material: cellulose materials saccharification is formed to fermentable sugars, and subsequent fermenting produces the beer containing ethanol.This technique proposes recycled fiber element enzyme and reuse them in further hydrolysis reaction.The people such as Chinese patent CN 101,899,488 A(Wan Yinhua) process for purification of sugar in a kind of lignocellulose enzymolysis liquid disclosed.The people such as Wan Yinhua have also proposed the method that high concentration ethanol is produced in the coupling of a kind of lignocellulose and membrane sepn, open by Chinese patent CN 102,174,593 A people such as () Wan Yinhua.But these correlative studys are all that comparatively gentle enzymic hydrolysis is carried out, and the more harsh chemical hydrolysis of condition are not carried out the research of reaction and separation processes coupling.Enzymic hydrolysis has reaction conditions gentleness, environmental friendliness, single-minded, the sugared yield advantages of higher of product, but zymin productive expense costliness, hydrolysis cycle are long, raw material needs the deficiencies such as pre-treatment to make biomass enzymic hydrolysis will reach technology and feasibility is economically had got long long way to go.
Chemical hydrolysis mainly refers to acid hydrolysis.Compare cellulase hydrolysis, acid hydrolysis has the advantages such as cost is low, easily-controlled reaction conditions.U.S. Patent No. 4,421,856 (people such as Muller) disclose a kind of method of producing ethanol: utilize acid hydrolysis to be hydrolyzed the aqueous slurry from starch or Mierocrystalline cellulose carbohydrate polymer, then ferment and distill, the stillage of distillation is hydrolyzed as feedstock recycle.The people such as Sakakit (Energy Fuels.1996.10:684-688) disclose a kind of conversion technology of surpass/near-critical water hydrocellulose fermentable sugars processed.The method hydrolysis effect is very good, but the rate of decomposition of fermentable sugars is also very large under hot conditions, and hydrolysate continues degraded, has a strong impact on the yield of fermentable sugars.Continue degraded for hydrolysate, the Li Yan of this seminar people such as rich grade (biomass chemical engineering, 2010,44 (1): 14-18.) has proposed glucose and in water-ethanol binary mixed solvent, has had good stability.Add ethanol to protect hydrolysate, although there is certain active effect, fail fundamentally to solve this difficult problem.
Membrane sepn is a novel isolation technique, and development in recent years is rapid, in industrial application and scientific research, obtains extensive concern.Membrane sepn process take pressure difference as impellent mainly comprises micro-filtration, ultrafiltration, nanofiltration and reverse osmosis; Mould material can be divided into organic membrane and mineral membrane, in the majority with organic high molecular layer, be used widely, but for exacting terms such as high temperature, high pressure, corrodibility are strong, organic membrane is because the limitation of its material can not meet the demands, and mineral membrane is compared with organic membrane, have high temperature resistant, resistance to chemical attack, resistance to bacterium and intensity advantages of higher, can make up the deficiency of organic membrane, meet exacting terms more, membrane separation technique is more widely used.
Summary of the invention
Technical problem to be solved by this invention is that a kind of method of utilizing membrane sepn and lignocellulose acid hydrolysis coupling to improve reducing sugar yield is provided for above-mentioned prior art, it is coupled hydrolysis reaction and membrane sepn, realize the timely separation of hydrolysate, avoid hydrolysate to continue degraded, thereby improve the yield of reducing sugar, the method organically combines common filtration, micro-filtration and ultrafiltration to use, effectively alleviate the pollution of hydrolyzed solution to ultra-filtration membrane, improved substrate conversion efficiency and reducing sugar yield.
The present invention solves the problems of the technologies described above adopted technical scheme, utilizes membrane sepn and lignocellulose acid hydrolysis coupling to improve the method for reducing sugar yield, it is characterized in that including following steps:
1) acid hydrolysis of lignocellulose: by acidic solution hydrolysis of lignocellulose, obtain hydrolyzed solution;
2) common filtration: step 1) gained hydrolyzed solution, by filtering, is obtained to the liquid that sees through of lignocellulose-containing small-particle, high glycan and reducing sugar, and the lignocellulose macroparticle of holding back is stayed in reactor and continued to be hydrolyzed;
3) micro-filtration filters: by step 2) liquid that sees through that obtains filters by micro-filtration, obtains the liquid that sees through containing high glycan and reducing sugar, and the lignocellulose small-particle of holding back returns to reactor and continues hydrolysis;
4) ultra-filtration filters: what step 3) was obtained sees through liquid by ultra-filtration filters, obtains the liquid that sees through containing reducing sugar, and the high glycan of holding back returns to reactor and continues hydrolysis.
Press such scheme, the lignocellulose described in step 1) can be wheat stalk, rice straw, maize straw, careless class or hardwood wood chip.
Press such scheme, the acidic solution described in step 1) can be sulfuric acid, hydrochloric acid, nitric acid, formic acid or toxilic acid.
Press such scheme, the acid hydrolysis temperature described in step 1) is 0 ~ 300 ℃, and pressure is 0 ~ 10 MPa, and in acidic solution, the massfraction of acid is 0.01% ~ 0.1%.
Press such scheme, step 2) described common filtration employing 200 ~ 1000 order stainless steel filtering nets filtrations, stainless steel filtering net is located at the outlet of hydrolyzed solution.
Press such scheme, the filter membrane mean pore size that micro-filtration described in step 3) adopts is 0.1 ~ 1 μ m, described filter membrane adopts organic membrane or inorganic ceramic, and the kit form of described filter membrane is rolling organic membrane assembly, tubular type organic membrane assembly, plate and frame organic membrane assembly or tubular type inorganic membrane assembly.
Press such scheme, described organic membrane is polysulfones, polyether sulphone, tetrafluoroethylene or polyvinylidene difluoride (PVDF).
Press such scheme, the molecular weight cut-off of the ultra-filtration membrane that the ultrafiltration described in step 4) adopts is 1000 ~ 10000 dalton, described ultra-filtration membrane adopts organic membrane or inorganic ceramic, and the kit form of described ultra-filtration membrane is rolling organic membrane assembly, tubular type organic membrane assembly, plate and frame organic membrane assembly or tubular type inorganic membrane assembly.
Press such scheme, described organic membrane is polysulfones, polyether sulphone, tetrafluoroethylene or polyvinylidene difluoride (PVDF).
The method that lignocellulose acid hydrolysis provided by the invention and membrane sepn coupling improve reducing sugar yield compared with prior art has the following advantages:
1) realize the hydrolysis of lignocellulose and separating of hydrolysate simultaneously;
2) make hydrolysate cooling in time, avoided the continuation degraded of hydrolysate;
3) the hydrolysate purity of gained is high, is conducive to follow-up conversion;
4) common filtration, micro-filtration and ultrafiltration are organically combined and used, effectively alleviated the pollution of hydrolyzed solution to filtering membrane.
Accompanying drawing explanation
Fig. 1 is be coupled the outward schematic flow sheet of the wherein a kind of mode that improves reducing sugar yield of lignocellulose acid hydrolysis of the present invention and membrane separation reactor;
Fig. 2 is the modified flow schematic diagram of Fig. 1;
Fig. 3 is the schematic flow sheet that in lignocellulose acid hydrolysis and membrane separation reactor, coupling improves the another kind of mode of reducing sugar yield;
Fig. 4 is the sectional structure chart of common filtration in Fig. 3, micro-filtration, ultrafiltration composite tube type membrane module;
In figure, 1. reactor 2. plain gauze 3. hydrolyzed solution outlet valve 4. cooling tank 5. micro-filtration fresh feed pump 6. micro-filtration membrane module 7. container for storing liquid 8. container for storing liquid outlet valve 9. ultrafiltration fresh feed pump 10. hyperfiltration membrane assembly 11. intake valve 12. reactor tapping valve 13. composite tube type membrane modules.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described in detail, but this explanation can not be construed as limiting the invention.
Embodiment 1:
Implementation step is as follows:
(1) press flow operations shown in Fig. 1, taking 30g particle diameter is that 180 object rice straws add in reactor 1, add sulphuric acid soln 450 ml of massfraction 0.05% by 1:15 solid-to-liquid ratio (g/ml), open intake valve 11 and be pressurized to 1.6 MPa, 200 ℃ of temperature, under stir speed (S.S.) 500 r/min conditions, react, the hydrolyzed solution outlet of reactor bottom arranges plain gauze 2, plain gauze is 500 object stainless steel filtering nets, gained hydrolyzed solution filters by plain gauze, obtain lignocellulose-containing small-particle, high glycan and reducing sugar see through liquid, the lignocellulose macroparticle of holding back is stayed in reactor and is continued to be hydrolyzed,
(2) open hydrolyzed solution outlet valve 3 and micro-filtration fresh feed pump 5, making step 2) liquid that sees through that obtains is cooled to rapidly room temperature through cooling tank 4, enter plate and frame micro-filtration membrane module 6, mould material is polysulfones, the mean pore size of filter membrane is 0.5 μ m, obtains the liquid that sees through containing high glycan and reducing sugar, and the lignocellulose small-particle of holding back returns to reactor and continues hydrolysis, see through liquid and enter container for storing liquid 7, simultaneously to feed supplement in reactor;
(3) open container for storing liquid outlet valve 8 and ultrafiltration fresh feed pump 9, make the liquid that sees through that step 3) obtains enter the daltonian plate and frame hyperfiltration membrane assembly 10 of molecular weight cut-off 10000, mould material is polysulfones, obtain the liquid that sees through containing reducing sugar, the high glycan of holding back returns to reactor and continues hydrolysis, collects the liquid that sees through containing reducing sugar.
(4) analysed preparation.
(5) there is a deficiency in the implementation case: because the stainless steel of reactor bottom is easily collected reactant small-particle, bring very large inconvenience to the cleaning of reactor.
Embodiment 2:
Implementation step is as follows:
(1) for solving the deficiency in embodiment 1, be convenient to reactor to clear up, the flow process of embodiment 1 is improved, change the installation site of stainless steel filtering net, as shown in Figure 2.
(2) press flow operations shown in Fig. 2, taking 30g particle diameter is that 180 object rice straws add in reactor 1, add sulphuric acid soln 450 ml of massfraction 0.05% by 1:15 solid-to-liquid ratio (g/ml), open intake valve 11 and be pressurized to 1.6 MPa, 200 ℃ of temperature, under stir speed (S.S.) 500 r/min conditions, react, reactor middle part arranges hydrolyzed solution outlet, outlet is wrapped up by plain gauze 2, plain gauze is 500 order stainless steel filtering nets, gained hydrolyzed solution is by common membrane filtration, obtain lignocellulose-containing small-particle, high glycan and reducing sugar see through liquid, the lignocellulose macroparticle of holding back is stayed in reactor and is continued to be hydrolyzed,
(3) open hydrolyzed solution outlet valve 3 and micro-filtration fresh feed pump 5, making step 2) liquid that sees through that obtains is cooled to rapidly room temperature through cooling tank 4, enter plate and frame micro-filtration membrane module 6, mould material is polysulfones, mean pore size is 0.5 μ m, obtains the liquid that sees through containing high glycan and reducing sugar, and the lignocellulose small-particle of holding back returns to reactor and continues hydrolysis, see through liquid and enter container for storing liquid 7, simultaneously to feed supplement in reactor.
(4) open container for storing liquid outlet valve 8 and ultrafiltration fresh feed pump 9, what make that step 3) obtains seeing through liquid enters the daltonian plate and frame hyperfiltration membrane assembly 10 of molecular weight cut-off 10000, and mould material is polysulfones.The high glycan of holding back returns to reactor and continues hydrolysis, collects the liquid that sees through containing reducing sugar.
(5) reaction finishes, and opens reactor tapping valve 12, discharge reaction residue, and water cleans up from the outlet of reactor bottom.
(6) analysed preparation.
Embodiment 3:
Concrete steps are as follows:
(1) press flow operations shown in Fig. 3, taking 30 g particle diameters is that 180 object rice straws add in reactor 1, add sulphuric acid soln 450 ml of massfraction 0.05% by 1:15 solid-to-liquid ratio (g/ml), open intake valve 11 and be pressurized to 1.6 mpa, 200 ℃ of temperature, under mixing speed 500 r/min conditions, react.
(2) hydrolyzed solution outlet is set at the middle part of reactor, outlet is made up of composite tube type membrane module 13, it is respectively common filtration 14 from outside to inside, microfiltration membrane 15 and ultra-filtration membrane 16, the common 500 order stainless (steel) wires that are filtered into, microfiltration membrane is 0.5 μ m inorganic ceramic film, ultra-filtration membrane is that molecular weight cut-off is 10000 daltonian inorganic ceramic films, open hydrolyzed solution outlet valve 3, hydrolyzed solution is successively by common filtering membrane, microfiltration membrane, ultra-filtration membrane flows out reactor, the lignocellulose macroparticle of holding back, lignocellulose small-particle and high glycan are stayed in reactor and are continued to be hydrolyzed, the liquid that sees through that contains reducing sugar is cooled to room temperature in time through cooling tank 4, collect and should see through liquid, simultaneously to feed supplement in reactor.
(3) reaction finishes, and opens reactor tapping valve 12, discharge reaction residue, and water cleans up from the outlet of reactor bottom.
(4) analysed preparation.
The analytical results of embodiment of the present invention 1-3:
Compare with the hydrolysate that adopts common batch still to react gained under the same terms, can obtain: concentration of reduced sugar adopts DNS colorimetry to measure, and embodiment 1: reducing sugar yield reaches 42.5 %, has improved 12.45 %; Embodiment 2: reducing sugar yield reaches 42.8%, has improved 12.75%; Embodiment 3: reducing sugar yield reaches 42%, has improved 11.95%.Hydrolysate is measured by high performance liquid chromatography, and result shows that the peak area of glucose increases, and the peak area of the oligose such as cellobiose, procellose reduces, and illustrates that polysaccharide is hydrolyzed to monose more, has improved reducing sugar yield.Hydrolysate degradation by-products is carried out GC-MS analysis, and result shows that the relative peak area of degraded product furfural, the levulinic acid etc. of glucose significantly reduces, and illustrates that the method has effectively suppressed the continuation degraded of hydrolysate.
Claims (1)
1. utilize membrane sepn and lignocellulose acid hydrolysis coupling to improve the method for reducing sugar yield, it is characterized in that including following steps:
1) acid hydrolysis of lignocellulose: by acidic solution hydrolysis of lignocellulose, obtain hydrolyzed solution, described lignocellulose is wheat stalk, rice straw, maize straw, careless class or hardwood wood chip, described acid hydrolysis temperature is 200 ℃, pressure is 1.6 MPa, in acidic solution, the massfraction of acid is 0.01% ~ 0.1%, and the acid in described acidic solution is sulfuric acid, hydrochloric acid, nitric acid, formic acid or toxilic acid;
2) common filtration: step 1) gained hydrolyzed solution is passed through to filter, obtain the liquid that sees through of lignocellulose-containing small-particle, high glycan and reducing sugar, the lignocellulose macroparticle of holding back is stayed in reactor and is continued to be hydrolyzed, described common filtration adopts 200 ~ 1000 order stainless steel filtering nets to filter, stainless steel filtering net is located at the outlet of hydrolyzed solution, is positioned at reactor middle part;
3) micro-filtration filters: by step 2) liquid that sees through that obtains filters by micro-filtration, obtains the liquid that sees through containing high glycan and reducing sugar, and the lignocellulose small-particle of holding back returns to reactor and continues hydrolysis; The filter membrane mean pore size that described micro-filtration adopts is 0.1 ~ 1 μ m, and described filter membrane adopts organic membrane or inorganic ceramic, and the kit form of described filter membrane is rolling organic membrane assembly, tubular type organic membrane assembly, plate and frame organic membrane assembly or tubular type inorganic membrane assembly; Described organic membrane is polyether sulphone, tetrafluoroethylene or polyvinylidene difluoride (PVDF);
4) ultra-filtration filters: the liquid that sees through that step 3) is obtained passes through ultra-filtration filters, obtain the liquid that sees through containing reducing sugar, the high glycan of holding back returns to reactor and continues hydrolysis, the molecular weight cut-off of the ultra-filtration membrane that described ultrafiltration adopts is 1000 ~ 10000 dalton, described ultra-filtration membrane adopts organic membrane or inorganic ceramic, the kit form of described ultra-filtration membrane is rolling organic membrane assembly, tubular type organic membrane assembly, plate and frame organic membrane assembly or tubular type inorganic membrane assembly, and described organic membrane is polyether sulphone, tetrafluoroethylene or polyvinylidene difluoride (PVDF).
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