CN103194505A - Enzyme hydrolysis saccharification method for furfural residue pretreatment by using green liquor - Google Patents
Enzyme hydrolysis saccharification method for furfural residue pretreatment by using green liquor Download PDFInfo
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Abstract
The invention relates to an enzyme hydrolysis saccharification method for furfural residue pretreatment by using green liquor. The enzyme hydrolysis saccharification method comprises the following steps of: preprocessing the furfural residue, carrying out enzyme hydrolysis saccharification on the furfural residue after preprocessing, wherein the preprocessing process comprises the following steps of: firstly, adopting a complexing agent to carry out chelation process on the green liquor, and then adding the green liquor after the chelation process and an oxidizing agent in the furfural residue so as to preprocess. The method provided by the invention has the advantages that the hydrolyzing efficiency is high, the cost is low, the process is simple, and the enzyme hydrolysis saccharification method is environment-friendly and is suitable for industrialized application.
Description
Technical field
The present invention relates to furfural dregs hydrolysis and saccharification field, be specifically related to a kind of enzymic hydrolysis method for saccharifying that adopts the pretreated furfural dregs of green liquor.
Background technology
In recent years; oil as the world economy pillar; because it is non-renewable, the factors such as ununiformity of the limitation of production technique, distribution have caused the whole world to face the worry of " oil crisis ", a series of is that the product of feedstock production also is faced with raw material supplying anxiety, the surging predicament of price with Sweet natural gas and oil.The utilization of simultaneously a large amount of petrochemical industry resources has caused beyond measure influence to environment, is directly threatening the safety of human health and life.For solving above-mentioned a series of problem, people transfer to eye on tellurian renewable resources-lignocellulose raw material gradually.Be that raw material can become glucose with cellulose conversion by enzymic hydrolysis with the lignocellulose material, can be converted into liquid fuel and industrial chemicals such as ethanol, butanols, lactic acid, acetone, glycerine through fermentation, can substitute the part petroleum resources, not only can make the mankind break away from undue dependence to petroleum resources, and can significantly reduce and pollute and the discharging of greenhouse gases.Furfural dregs is the waste that produces in the furfurol industry production process, and furfural product per ton is discharged residue more than 10 tons, about 3,000 ten thousand tons of China's annual discharging furfuraldehyde waste slag.These waste residues except small part by direct reuse in boiler combustion, adopt at present mostly the method for piling up or digging pit and toppling over, both wasted resource, polluted environment, taken a large amount of soils again, become the bottleneck of the sector development gradually.Contain a large amount of Mierocrystalline celluloses and xylogen in the furfural dregs, wherein content of cellulose surpasses 45%, and this part Mierocrystalline cellulose can directly or carry out cellulase hydrolysis after pre-treatment, produces alcohol fuel or other chemical by the mode of fermentation.
Substitute oil as the technical study of fuel comparative maturity with preparing ethanol from wood fiber raw material, yet because economical efficiency, fail large-scale commercial production.Reason mainly contains two aspects: the one, and the enzyme dosage that the sexual needs of stubbornly resisting that lignocellulose raw material is natural are more and the preprocessing process of higher-strength have increased production cost; The 2nd, the xylogen in the lignocellulose raw material greatly reduces enzyme active principle concentration to the ineffective adsorption of cellulase.The software engineering researchers invent of various countries diverse ways attempt to solve above-mentioned bottleneck, raw material is carried out the accessibility that pre-treatment improves cellulase, be the focus and emphasis of research at present.Pretreatment method of wood fiber raw materials mainly contains: physics method, acid treatment, alkaline purification, oxidation, Biological Pretreatment; In addition, add the transformation efficiency that tensio-active agent can improve enzyme, reduce the requirement of enzyme.The production of furfural is to carry out under the diluted acid condition of heat, and lignin under high temperature, acidic conditions condensation can take place, so the lignin in the furfural dregs mainly is acid soluble lignin.The research report is after acid soluble lignin absorption, and the activity of cellulase can reduce more than 90%, and therefore the lignin of removing as far as possible in the raw material is the method that effectively improves cellulase hydrolysis efficient.Alkaline process (NaOH method) preconditioning technique is to be commonly used to be used widely on pulp and paper industry as the pretreated method of biomass material.But adopt alkaline process that furfural dregs is carried out pre-treatment, can not effectively remove the acid soluble lignin in the furfural dregs, and bigger degraded can take place Mierocrystalline cellulose under the high-temperature alkaline condition.After adding hydrogen peroxide, the HOO that the hydrogen peroxide hydrolysis produces
-Can effectively degrade lignin in the furfural dregs makes the lignin stripping, thereby can improve the hydrolysis efficiency of cellulase, and the pretreated temperature of alkaline hydrogen peroxide is lower than 100 ℃ in addition, can reduce cellulosic degraded, is a kind of potential industrial process therefore.
After pre-treatment finished, the solid ingredient of rich cellulose can directly be used for carrying out enzymic hydrolysis and produce glucose through washing.Contain a large amount of organism (mainly being low-molecular-weight lignin degradation products) in the liquid after the washing, and the material of the remaining pharmaceutical chemicals of preprocessing process and low molecular degradation thing and reactant generation.Because washings is black, on pulp and paper industry this part liquid is called " black liquor ", directly is put into and causes serious environmental to pollute in the water body.Utilization to black liquor mainly is that heat is reclaimed in its burning at present, idiographic flow is: rare black liquor carries out the above moisture of evaporation concentration to 90% and is removed, black liquor after will concentrating again sprays in the alkali recovery boiler thorax and burns, and the heat that burning produces can be used for producing or generating.The main composition of remaining melts of burning is inorganic salt, and the back liquid that is dissolved in water is green and (contains small amount of Fe
2+), be called " green liquor ".The green liquor main component that adopts sodium hydroxide method slurrying to produce is NaOH and Na
2CO
3, if carry out industrial production with the alkaline hydrogen peroxide method for pretreating, also mainly contain above-mentioned two kinds of compositions in the green liquor of generation.
Summary of the invention
The lower defective of efficient when overcoming furfural dregs enzymic hydrolysis saccharification the purpose of this invention is to provide a kind of enzymic hydrolysis method for saccharifying of furfural dregs.
The enzymic hydrolysis method for saccharifying of furfural dregs provided by the invention is: earlier furfural dregs is carried out pre-treatment, then pretreated furfural dregs is carried out the enzymic hydrolysis saccharification, wherein, described preprocessing process comprises: at first adopt complexing agent that green liquor is carried out chelation treatment, then the green liquor after the chelation treatment and oxygenant are joined in the furfural dregs together it is carried out pre-treatment.
Wherein, in the described chelation treatment step, the usage quantity of complexing agent is 0.1～5% of green liquor weight by weight, preferred 0.5～2%.
Wherein, the time of described chelation treatment is 0.1～3 hour.
Wherein, in the described pre-treatment step, the green liquor after the chelation treatment: oxygenant: the furfural dregs solid substance is 1～10: 0.1～1.0: 1(ml: g: g).
Wherein, the described pretreated time is 2～8 hours, and temperature is 60～120 ℃.
Wherein, to be washed to the pH value before carrying out pre-treatment be 6～7 to described furfural dregs.
Wherein, in the described enzymic hydrolysis saccharification, the consumption of cellulase is 15～25FPU/g substrate.Preferably, in the described enzymic hydrolysis saccharification, hydrolysis time is 50～100h, and hydrolysis temperature is 40～60 ℃.
Technical scheme provided by the invention has the following advantages:
(1) pre-treatment of adopting green liquor-oxygenant to be coupled to furfural dregs, can improve the hydrolysis efficiency of cellulase, and lower in the cellulosic loss of preprocessing process, the chemical cost amount is also lower, compare with the preprocessing process that adopts highly basic-oxygenant coupling, can save the cost more than 30%.
(2) add complexing agent green liquor is carried out chelation treatment, complexing agent can reduce in green liquor and the furfural dregs metal ion to the consumption of oxygenant, also can reduce metal ion influence to cellulase activity in enzymolysis process, thereby improve the hydrolysis efficiency of cellulase.
(3) preprocessing process uses the green liquor of generations such as pulping and paper-making factory, provides foundation to energy consumption height, with serious pollution enterprises in pulp and paper industry development new bio refining industrial system, has alleviated the environmental stress of green liquor discharging.
(4) pretreatment technology is simple, is easy to realization and existing industry and has favorable compatibility.
(5) the green liquor participation pre-treatment capable of circulation of furfural dregs enzymic hydrolysis recovery, thus the recycling of realization partial material has reduced production cost, has also further reduced the environmental pollution that discharging of waste liquid brings.
Description of drawings
Fig. 1 is the process flow sheet of the method for the invention.
Embodiment
The enzymic hydrolysis method for saccharifying of the pretreated furfural dregs of green liquor that embodiment of the present invention provides may further comprise the steps: earlier furfural dregs is carried out pre-treatment, then pretreated furfural dregs is carried out the enzymic hydrolysis saccharification.
Preprocessing process wherein comprises: at first adopt complexing agent that green liquor is carried out chelation treatment, then the green liquor after the chelation treatment and oxygenant are joined in the furfural dregs together it is carried out pre-treatment.
In the above-mentioned preprocessing process, utilize highly basic and oxygenant acting in conjunction in the green liquor that furfural dregs is carried out pre-treatment, green liquor is with low cost, can obviously reduce the cost of furfural dregs hydrolysis and saccharification, but also has alleviated the environmental stress that the green liquor discharging brings.
Employed green liquor wide material sources wherein, as common field of papermaking, technology of the present invention can be directly and the coupling of pulping and paper-making production line form large-scale production.Except from the common industrial circle, green liquor can also be from the black liquor behind the furfural dregs hydrolysis and saccharification, with after its burning namely, can realize the recycle of material, further to reduce production costs.
In the chelation treatment step, the usage quantity of complexing agent can be determined according to the metal ion content situation in green liquor and the furfural dregs, in general, is 0.1～5% of green liquor weight by weight, preferred 0.5～2%.
In the green liquor except containing available highly basic, also contain a large amount of metal ions, especially the metal ion of divalence or trivalent, can consume a large amount of oxygenants, and also can have a negative impact to the enzymolysis of cellulase, make the transformation efficiency of sugar lower, in addition, also contain the metal ion of influential enzymolysis in the furfural dregs, further restricted transformation efficiency.In the chelation treatment step, make the metal ion in itself and the green liquor carry out chelating by adding complexing agent, thereby reduce metal ion to the consumption of oxygenant, also can reduce in the follow-up hydrolysis and saccharification step metal ion to the influence of cellulase, by the chelation treatment step, can reduce the cost of enzymic hydrolysis saccharification, improve the transformation efficiency of enzymic hydrolysis saccharification.
Wherein, complexing agent can use any can with green liquor, furfural dregs in metal ion carry out the complexing agent of chelating, preferred complexing agent is EDTA.
In the chelation treatment step, the time of processing is 0.1～3 hour, preferred 0.5～2 hour.
In the above-mentioned pre-treatment step, the green liquor after the chelation treatment: oxygenant: the furfural dregs solid substance is 1～10: 0.1～1.0: 1(ml: g: g); Preferred 5～10: 0.1～0.5: 1(ml: g: g).
In the above-mentioned pre-treatment step, the pretreated time is 2～8 hours, and temperature is 60～120 ℃.Preferably, the pretreated time is 2～4 hours, and temperature is 70～100 ℃.
In the above-mentioned pre-treatment step, oxygenant can be selected inorganic oxidizer commonly used for use, preferred hydrogen peroxide.
In the above-mentioned pre-treatment step, furfural dregs was washed to the pH value before handling be 6～7.
In the above-mentioned enzymic hydrolysis saccharification step, the consumption of cellulase is 15～25FPU/g Mierocrystalline cellulose.
In the above-mentioned enzymic hydrolysis saccharification step, hydrolysis time is 50～100h, and hydrolysis temperature is 40～60 ℃.
As shown in Figure 1, the enzymic hydrolysis method for saccharifying detailed process that embodiment of the present invention provides is as follows: get furfural dregs and wash, filter, get the pH value and approach neutral filter residue, add water again and be adjusted to finite concentration; Add metal chelating agent such as EDTA in the green liquor and carry out chelation treatment, oxygenants such as the green liquor after the chelation treatment and hydrogen peroxide are joined together the pre-treatment of carrying out certain hour in the furfural dregs after the aforementioned processing; Pretreated furfural dregs is washed till neutrality, filters, collect filtrate and filter residue, filter residue is adjusted to finite concentration, add the cellulase saccharification that is hydrolyzed; Filtrate is black liquor, the generation heat energy that can burn after concentrating, and the melts after the burning is dissolved in water and namely gets green liquor, can continue to drop in the pre-treatment of furfural dregs to realize the recycle of material.
The furfural dregs that embodiment of the present invention is used is the common industrial furfural dregs, and water content is about 55-60%, and the pH value is about 2-3.
The green liquor that embodiment of the present invention is used is taken from the paper mill, by the quality solid content be about 10%, carbonate content is about 7.5%, sodium hydrate content is 2.3%.
The oxygenant that embodiment of the present invention is used is preferably commercially available hydrogen peroxide, and hydrogen peroxide massfraction wherein is 30%.
The cellulase that embodiment of the present invention is used is the commercially available cellulase that can be used for the disposable type of furfural dregs hydrolysis and saccharification.
The reagent that does not further specify in the embodiment of the present invention, operation etc. are this area routine techniques.
Embodiment 1
Get furfural dregs and add water and be adjusted to solid content and be about 10wt%, soak 24h, intermittently stir, filter, filter residue is 6-7 until pH 3-5 time with the tap water flushing again, the filter residue dry for standby.
Adding massfraction is that 0.5%(is with respect to filtrate) EDTA among green liquor, stir 2.5h to mix the green liquor after the chelation treatment.
Green liquor after the chelation treatment and hydrogen peroxide (30%) and above-mentioned furfural dregs filter residue are joined in the pressure bottle together.The add-on of green liquor is 6ml/(g furfural dregs filter residue), the add-on of hydrogen peroxide is 0.6g/(g furfural dregs filter residue), add water and adjust solid content and be about 3.3wt%.Pressure bottle is heated to 80 ℃ in the shaking bath of 150rpm, and is incubated 3h under identical condition, pre-treatment finishes after the 3h.
Pretreated furfural dregs wash with water to pH be 6-7, filter, collection filtrate is black liquor.The furfural dregs solid quality percentage concentration that adds in the filter residue after the water adjustment is handled is about 2.5%, adds the 18FPU/(g Mierocrystalline cellulose) the cellulase saccharification that is hydrolyzed, hydrolysis temperature is 48 ℃, the pH value is 4.8, conversion coefficient is 87.9% behind the hydrolysis 96h.Lignin content is reduced to 17.8% by quality (with respect to the furfural dregs raw material solid) by 45.3%, and content of cellulose is reduced to 40.7% by quality (with respect to the furfural dregs raw material solid) by 45.9%.
Embodiment 2
Get furfural dregs and add water and be adjusted to solid content and be about 10wt%, soak 24h, intermittently stir, filter, filter residue is 6-7 until pH 3-5 time with the tap water flushing again, the filter residue dry for standby.
Adding massfraction is that 1%(is with respect to filtrate) EDTA in green liquor, stir 1.5h to mix the green liquor after the chelation treatment.
Green liquor after the chelation treatment and hydrogen peroxide (30%) and above-mentioned furfural dregs filter residue are joined in the pressure bottle together.The add-on of green liquor is 7ml/(g furfural dregs filter residue), the add-on of hydrogen peroxide is 0.5g/(g furfural dregs filter residue), add water and adjust solid content and be about 3.5wt%.Pressure bottle is heated to 75 ℃ in the shaking bath of 150rpm, and is incubated 3.5h under identical condition, pre-treatment finishes after the 3.5h.
Pretreated furfural dregs wash with water to pH be 6-7, filter, collection filtrate is black liquor.Adding water in the filter residue adjusts pretreated furfural dregs concentration and is about 3.0%(w/v), add the 15FPU/(g Mierocrystalline cellulose) the cellulase saccharification that is hydrolyzed, hydrolysis temperature is 50 ℃, the pH value is 4.8, conversion coefficient is 90.4% behind the hydrolysis 96h.Lignin content is reduced to 16.9% by quality (with respect to the furfural dregs raw material solid) by 44.7%, and content of cellulose is reduced to 40.1% by quality (with respect to the furfural dregs raw material solid) by 46.2%.
Embodiment 3
Get furfural dregs and add water and be adjusted to solid content and be about 10wt%, soak 24h, intermittently stir, filter, filter residue is 6-7 until pH 3-5 time with the tap water flushing again, the filter residue dry for standby.
Adding massfraction is that 1.5%(is with respect to filtrate) EDTA in green liquor, stir 1.0h to mix the green liquor after the chelation treatment.
Green liquor after the chelation treatment and hydrogen peroxide (30%) and above-mentioned furfural dregs filter residue are joined in the pressure bottle together.The add-on of green liquor is 5.5ml/(g furfural dregs filter residue), the add-on of hydrogen peroxide is 0.8g/(g furfural dregs filter residue), add water and adjust solid content and be about 2.5wt%.Pressure bottle is heated to 100 ℃ in the shaking bath of 220rpm, and keeps 2.5h under identical condition, pre-treatment finishes after the 2.5h.
Pretreated furfural dregs wash with water to pH be 6-7, filter, collection filtrate is black liquor.Adding water in the filter residue, to adjust pretreated furfural dregs concentration be 2.2%(w/v), add the 20FPU/(g Mierocrystalline cellulose) the cellulase saccharification that is hydrolyzed, hydrolysis temperature is 45 ℃, the pH value is 5.0, conversion coefficient is 90.1% behind the hydrolysis 96h.Lignin content is reduced to 15.6% by quality (with respect to the furfural dregs raw material solid) by 47.1%, and content of cellulose is reduced to 39.2% by quality (with respect to the furfural dregs raw material solid) by 46.7%.
Comparative Examples 1
Do not carry out pre-treatment, the saccharification that directly furfural dregs is hydrolyzed, all the other steps are with embodiment 1, and the conversion coefficient after the hydrolysis is 71.3%.
Comparative Examples 2
Carry out pre-treatment, but green liquor does not carry out chelation treatment, all the other steps are with embodiment 1, and the conversion coefficient after the hydrolysis is 78.3%.Lignin content (with respect to the furfural dregs raw material) is reduced to 27.6% by 45.3%, and content of cellulose (with respect to the furfural dregs raw material) is reduced to 45.6% by 45.9%.
Comparative Examples 3
Carry out pre-treatment, but green liquor does not carry out chelation treatment, all the other steps are with embodiment 2, and the conversion coefficient after the hydrolysis is 82.7%.Lignin content (with respect to the furfural dregs raw material) is reduced to 24.3% by 45.3%, and content of cellulose (with respect to the furfural dregs raw material) is reduced to 43.4% by 45.9%.
Comparative Examples 4
Carry out pre-treatment, but green liquor does not carry out chelation treatment, all the other steps are with embodiment 3, and the conversion coefficient after the hydrolysis is 83.6%.Lignin content (with respect to the furfural dregs raw material) is reduced to 21.4% by 45.3%, and content of cellulose (with respect to the furfural dregs raw material) is reduced to 42.1% by 45.9%.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the enzymic hydrolysis method for saccharifying of the pretreated furfural dregs of green liquor, earlier furfural dregs is carried out pre-treatment, then pretreated furfural dregs is carried out the enzymic hydrolysis saccharification, it is characterized in that, described preprocessing process comprises: at first adopt complexing agent that green liquor is carried out chelation treatment, then the green liquor after the chelation treatment and oxygenant are joined in the furfural dregs together it is carried out pre-treatment.
2. method according to claim 1 is characterized in that, in the described chelation treatment step, the usage quantity of complexing agent is 0.1～5% of described green liquor weight by weight; Preferred 0.5～2%.
3. method according to claim 1 and 2 is characterized in that, described complexing agent is EDTA.
4. according to each described method of claim 1-3, it is characterized in that the time of described chelation treatment is 0.1～3 hour.
5. according to each described method of claim 1-3, it is characterized in that in the described pre-treatment step, the green liquor after the chelation treatment: oxygenant: the furfural dregs solid substance is 1～10: 0.1～1.0: 1(ml: g: g).
6. method according to claim 5 is characterized in that, the described pretreated time is 2～8 hours, and temperature is 60～120 ℃.
7. according to each described method of claim 1-3, it is characterized in that described oxygenant is hydrogen peroxide.
8. according to each described method of claim 1-3, it is characterized in that it is 6～7 that described furfural dregs was washed to the pH value before handling.
9. according to each described method of claim 1-3, it is characterized in that in the described enzymic hydrolysis saccharification step, the consumption of cellulase is 15～25FPU/g Mierocrystalline cellulose.
10. method according to claim 9 is characterized in that, in the described enzymic hydrolysis saccharification step, hydrolysis time is 50～100h, and hydrolysis temperature is 40～60 ℃.
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Application publication date: 20130710 |