CN104878055A - Method for pretreating ethyl alcohol produced from corn straws - Google Patents
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Abstract
The invention discloses a method for pretreating ethyl alcohol produced from corn straws. The method comprises the following steps: taking corn straws as a raw material, pulverizing the corn straws, and conducting air drying to obtain corn straw powder; balancing moisture in the corn straw powder, adding water and acid liquor, conducting slightly acidic medium pressure steam explosion pretreatment, after hydrolysis reaction is finished, conducting centrifugal separation on the exploded sample and hydrolysate, and separately collecting a sample a and a hydrolysate I; balancing moisture in the corn straw powder, conducting neutral steam explosion pretreatment, after hydrolysis reaction is finished, conducting centrifugal separation on the exploded sample and hydrolysate, and separately collecting a sample b and a hydrolysate II; washing the sample a and the sample b subjected to prehydrolysis to be clean, and mixing so as to obtain a cellulose substrate used for follow-up enzymolysis fermentation. According to the method, a scientific overall process is provided, the pretreated sample obtains excellent application effects on the aspect of ethyl alcohol preparation through enzyme hydrolysis, and certain technical guidance is provided for the engineering application of converting the corn straws into the biological ethyl alcohol.
Description
Technical field
The invention belongs to the technical field that cellulose raw material produces ethanol, especially relate to the pretreatment process that a kind of maize straw produces ethanol.
Background technology
Biomass are a kind of important renewable resourcess, and produce by it requirement that alcohol fuel meets environmental protection, Sustainable development, being the new forms of energy most possibly replacing oil, having huge development prospect, is also one of focus of current research.China's biomass material is very abundant; annual production about 11.45 hundred million tons, wherein stalk reaches more than 700,000,000 ton, and maize straw has accounted for 35%; if they to be changed into gas or liquid fuel, by crisis of resource, the series of problems such as energy shortage and environmental pollution alleviating the mankind effectively and face.But the lignocelluloses such as maize straw form network structure by Mierocrystalline cellulose, hemicellulose and xylogen by covalent bond, due to the crystalline texture of itself densification, it is very low directly to carry out enzymolysis efficiency, so must carry out pre-treatment.
At present, the pretreatment process of maize straw is broadly divided into Physical, chemical method and biological process.Physical mainly adopts the modes such as pulverizing, high-energy radiation, steam explosion to reduce cellulosic degree of crystallinity, improves its accessibility.Wherein pulverize and high-energy radiation energy consumption high, very little to the increase rate of enzymatic hydrolyzation.And steam explosion pre-treatment is a kind of effective pretreatment process, it mainly utilizes high temperature and high pressure steam, by abrupt release press process, realizes Component seperation and the structural changes of raw material.Steam explosion pre-treatment effectively can realize lignocellulose chemical composition and be separated, and uses no or little pharmaceutical chemicals, environmentally safe, and energy consumption is lower, is that development in recent years is than lignocellulose high efficient separation technology that is very fast, low cost.But this method generally needs to carry out at 200 ~ 230 DEG C, and pressure reaches 2 ~ 3MPa, high to operational requirement, limit the application of its through engineering approaches.According to dilute acid pretreatment lignocellulose, effectively by the oligopolymer that hydrolysis of hemicellulose is monose and solubility, thus cellulosic conversion can be improved, reduce pressure and the time of Steam explosion treatment.Chemical method mainly removes hemicellulose, lignin with acid, alkali, organic solvent etc., but seriously polluted to environment.Biological rule mainly adopts some microorganisms (mainly white-rot fungi, brown rot fungus, soft rotten fungi) lignin degrading.But these fermentable cycles are long, efficiency is low, cannot industrial production.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency overcoming existing cellulose raw material production alcohol pre-treatment technology, provides a kind of maize straw to produce the pretreatment process of ethanol.The inventive method is adopted can effectively to improve enzymolysis yield.
A kind of maize straw produces the New Pre treatment process of ethanol, take maize straw as raw material, neutrality and slightly acidic middle pressure steam explosion pre-treatment is carried out after being ground by maize straw, then comparative study is passed through, after showing that slightly acidic middle pressure steam explosion pre-treatment mixes with the pretreated product of neutral steam explosion, be conducive to the carrying out of follow-up enzyme digestion reaction.
Technical scheme of the present invention is as follows:
Maize straw produces a pretreatment process for ethanol, and the concrete steps of the method are:
S1: get corn stalk raw material, mechanical disintegration to 3 ~ 5cm, be air-dryly in its natural state less than 5% ~ 10% to moisture, obtains maize straw powder, Air drying storage under ambient conditions, for subsequent use;
S2. prehydrolysis: by S1 step gained maize straw powder equilibrium water content, add water and acid solution, carry out slightly acidic middle pressure steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collect sample a and hydrolyzed solution respectively, for subsequent analysis;
S3. prehydrolysis: by S1 step gained maize straw powder equilibrium water content, carry out neutral steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collects sample b and hydrolyzed solution, respectively for subsequent analysis;
S4. the explosion sample obtained S2 and S3 carries out chemical composition analysis and morphological structure analysis, carries out sugar analysis to pre-hydrolyzed solution;
S5. collect the sample a after S2 and S3 prehydrolysis and sample b respectively, after washes clean, mix than for the ratio of 1:1 ~ 3:1 according to absolute dry mass, obtain the cellulosic substrate for follow-up enzymatic hydrolysis and fermentation.
In aforesaid method, described maize straw takes from the Northeast of China.
In aforesaid method, in S2, the pretreated condition of described slightly acidic middle pressure steam explosion is: concentration of substrate is 0 ~ 20%, and acid solution massfraction is 0 ~ 2%, and burstpressures is 0.8 ~ 1.0MPa, and the reaction times is 0 ~ 15min.
In aforesaid method, in S3, the pretreated condition of described neutral steam explosion is: concentration of substrate is 0 ~ 20%, and acid solution massfraction is 0%, and burstpressures is 0.8 ~ 1.0MPa, and the reaction times is 0 ~ 15min.
In aforesaid method, described acid solution is sulphuric acid soln.
In aforesaid method, analytical instrument is Olympus BX51 biomicroscope, Carl Zeiss EVO18 type scanning electronic microscope, IC 5000 ion chromatograph, Metso FS-300 automatic fibers analyser, MicroMeritics ASAP2020 full-automatic specific surface area pore analysis instrument and other conventional analytical instruments.
The invention has the beneficial effects as follows:
The present invention adopts slightly acidic middle pressure steam blasting technology to carry out pre-treatment to maize straw, and sulfuric acid dosage is few, and pretreating effect is high, is more conducive to reducing production cost, improves enzymolysis efficiency.
The present invention adopts slightly acidic middle pressure steam blasting technology to carry out pre-treatment to maize straw, while raising stalk sugar yield, remove the inhibited hemicellulose of fermenting process and a small amount of xylogen, produce for the clean and effective carrying out the products such as alcohol fuel further and provide an effective way.
Accompanying drawing explanation
Fig. 1 explosion pre-treatment is on the impact of Main chemical component relative content.
Fig. 2 a is that raw material SEM schemes; Fig. 2 b is that 1# steam explosion SEM schemes; Fig. 2 c is the acid explosion SEM figure of 2#.
Embodiment
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.Unless stated otherwise, the reagent that adopts of the present invention and raw material are the conventional commercial reagent in this area and raw material.Unless stated otherwise, the percentage ratio related in the embodiment of the present invention is mass percent.
Embodiment 1
Material choice: the present invention's maize straw used takes from the Northeast of China.
1. instrument:
Plant pulverizer, precision electronic balance, retort furnace, water-bath, air dry oven, vacuum pump using circulatory water, fast tester for water content, hot plate, DR5000 spectrophotometer, Soxhlet extractor.
2 raw materials and process:
Maize straw takes from Changchun, China Jilin, gets representative raw material at random, mechanical disintegration to 3 ~ 5cm, is air-dryly in its natural state less than 10% to moisture.Air drying storage under ambient conditions equilibrium water content in plastics bag, when analyzing bagasse chemical composition and pre-treatment for subsequent measurements.
3. result:
The chemical composition analytical results of the maize straw of described kind is listed in the table below in 1.
As can be seen from Table 1, this maize straw is also primarily of Mierocrystalline cellulose, hemicellulose (poly-pentose), lignin composition, these three parts account for 86% of raw material total mass, wherein holocellulose (comprising Mierocrystalline cellulose and hemicellulose) content is 68.53%, and these components can be converted into ethanol in theory; As for lignin, this component concentration is relatively high, and total content is 17.50%, because lignin is wrapped between Mierocrystalline cellulose and hemicellulose, therefore needs in preprocessing process, to make it peel off, fully to expose Mierocrystalline cellulose as far as possible.
Hot water extract and 1%NaOH extractum are all process raw material 60min at 100 DEG C, and therefore the number of extractum content can reflect degradation capability and the alkaline cooking yield of raw material to a certain extent.As can be seen from Table 1, hot water extract's content of maize straw be 20.07%, 1%NaOH extractum content more than 50%, corn stalk raw material easily processes as can be seen here, easily degrades under acid, alkali condition.
In addition, as can also be seen from Table 1, raw material also containing the ash content of 3.86%, the pectin of 1.73% and 1.58% tannin, these materials are a small amount of components in plant fiber material chemical composition.
The chemical composition of table 1 maize straw
Embodiment 2
The neutral steam explosion pre-treatment of maize straw
1. instrument:
Steam blasting device; Olympus BX51 biomicroscope; Carl Zeiss EVO18 type scanning electronic microscope; IC 5000 ion chromatograph; Metso FS-300 automatic fibers analyser; Micro MeriticsASAP2020 full-automatic specific surface area pore analysis instrument.
2. raw material and process:
By embodiment 1 gained maize straw powder equilibrium water content, carry out neutral steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collect sample and hydrolyzed solution respectively, for subsequent analysis (design parameter is in table 2); After process, by the sample of explosion and hydrolyzed solution centrifugation, filtrate for analysis carbohydrate components, after substrate puts into sealing plastics bag equilibrium water content, for analyzing yield.Then representative substrate sample is got, after natural air drying, for chemical composition analysis and fibre shape analysis.
Table 2 neutral explosion pretreatment technology condition
3. result:
3.1 hydrolysis sample chemical compositions are analyzed
By preceding method process hydrolysis sample, the sample chemical composition that is hydrolyzed analysis, acquired results is listed in table 3.
The chemical composition of table 3 neutral explosion pre-treatment sample
Note: absolute magnitude is the actual content of component in pre-treatment sample;
Relative quantity=absolute magnitude × hydrolysis yield;
As can be seen from the data of table 3, adopt Steam explosion treatment (1# sample), yield is relatively high, and remaining solid substance amount is 83.84%.The absolute content of each component from table 3, compared with untreated raw material, after process, the hemi-cellulose content of sample is on a declining curve, and content reduces to 17.02%.From lignin content, after explosion treatment, the lignin total amount of sample is also on a declining curve, and neutral steam explosion sample trees cellulose content reduces to 15.13%.And for acid soluble lignin, its content then increases to some extent, this illustrates that Steam explosion treatment can make part acid insoluble lignin be converted into acid soluble lignin.
3.2 neutral explosion pre-treatment are on the impact of carbohydrate components in pre-hydrolyzed solution
After the neutral steam explosion pre-treatment of maize straw, in pre-hydrolyzed solution, carbohydrate components change is as shown in table 4.
Table 4 neutral steam explosion pre-hydrolyzed solution carbohydrate components content
From the data of table 4, after Steam explosion treatment, the carbohydrate of degraded mainly exists with polysaccharide form, and its concentration reaches 7.03g/L, accounts for 94.4% of total sugar content.And polysaccharide mainly exists with the form of glucose, its concentration accounts for 69% of polysaccharide amount, is secondly pectinose and wood sugar.Monose is then based on pectinose and wood sugar, and glucose monosaccharide and galactose monosaccharide then do not detect.This is because as an acidic catalyst, water at high temperature can promote that hydrolysis of hemicellulose is the monose such as wood sugar.But due to the H of water extraction confession
+limited, usually need the higher quick-fried temperature of vapour, and wood sugar at high temperature can be decomposed into the fermentation inhibitor such as furfural, acetic acid further.
Embodiment 3
The slightly acidic middle pressure steam explosion pre-treatment of maize straw
1. instrument:
Steam blasting device; Olympus BX51 biomicroscope; Carl Zeiss EVO18 type scanning electronic microscope; IC 5000 ion chromatograph; Metso FS-300 automatic fibers analyser; Micro MeriticsASAP2020 full-automatic specific surface area pore analysis instrument.
2. raw materials pretreatment:
By embodiment 1 gained maize straw powder equilibrium water content, add water and acid solution, carry out slightly acidic middle pressure steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collect sample and hydrolyzed solution respectively, for subsequent analysis (parameter refers to table 5); After process, by the sample of explosion and hydrolyzed solution centrifugation, filtrate for analysis carbohydrate components, after substrate puts into sealing plastics bag equilibrium water content, for analyzing yield.Then representative substrate sample is got, after natural air drying, for chemical composition analysis and fibre shape analysis.
Table 5 slightly acidic explosion pretreatment technology condition
3. test result
3.1 hydrolysis sample chemical compositions are analyzed
By preceding method process hydrolysis sample, the sample chemical composition that is hydrolyzed analysis, gained test result is listed in table 6.
The chemical composition of table 6 acid explosion pre-treatment sample
Note: absolute magnitude is the actual content of component in pre-treatment sample;
Relative quantity=absolute magnitude × hydrolysis yield;
As can be seen from the data of table 6, adopt acid explosion treatment, remaining solid substance amount is 72.56%, illustrates that acid explosion treatment can the more material of stripping.The absolute content of each component from table 6, compared with untreated raw material, after process, the hemi-cellulose content of sample is on a declining curve, and acid explosion pre-treatment hemi-cellulose content reduces to 16.13%, shows that acid explosion more easily makes poly-pentose stripping.This is because sulfuric acid provides more H
+, H
+the hydrolysis of hemicellulose can be promoted as catalyzer.Have research to point out, dilute acid steam explosion synergy comprises activation two kinds of mechanism of the softening of diluted acid and steam explosion.Diluted acid can remove most hemicellulose, destroys the interaction between hemicellulose and lignin, thus softening fibre tissue.Steam explosion utilizes the pressure reduction of moment the Mierocrystalline cellulose supramolecular structure activated under high-temperature and high-pressure conditions " can be freezed ", and then is conducive to the contact of cellulase.From lignin content, after explosion treatment, the lignin total amount of sample is also on a declining curve, and acid explosion sample trees cellulose content reduces to 12.33%, shows that the lignin of acid explosion treatment stripping is more.
From relative content and the variation tendency of the neutral explosion of Fig. 1 and each component of acid explosion substrate, the content of holocellulose is maximum, and its value is reduced to 43.85% from 51.73%, decreases about 8%.For hemi-cellulose content, its value drops to 11.70% from 14.27%, reduces about 2.6%.For lignin content (comprising acid insoluble lignin and acid soluble lignin), its value is down to 8.94% from 12.69%, reduces about 3.8%.
The specific surface area of sample and aperture before and after table 7 explosion treatment
From the aperture of table 7, the aperture of acid explosion treatment substrate is about 19.36nm, and corresponding pore volume is also from the 0.001075cm by raw material
3/ g increases to 0.008510cm
3/ g, this is mainly because raw material mix is dense, and after acid explosion treatment, hole increases, and structure becomes loose.This also can find out from the result of Fig. 2 a-Fig. 2 c scanning electron microscope.Fig. 2 a-Fig. 2 c shows the stereoscan photograph of sample under raw material and different explosion treatment, can find out that untreated raw fibre surface compact is orderly from Fig. 2 a; After neutral explosion treatment (Fig. 2 b), fiber sheath starts to come off, and surface hole defect increases and high-visible; Through peracidity explosion treatment (Fig. 2 c), its structure deteriorate is obvious, and fiber sheath peels off further, gully is deepened, and occurred rupturing and large hole, the contact site of such Cellulase Molecules and substrate will be improved greatly, thus after making enzymolysis, reducing sugar yield improves.
Staple length, width, the fines content of table 8 explosion treatment sample
Table 8 shows the change of the staple length of sample after explosion treatment, width and tiny component.As can be seen from Table 8, the staple length of two samples after explosion treatment all increases, this is mainly owing to tissue stripping after explosion treatment that the medulla, leaf etc. of maize straw are formed primarily of heteroproteose cell, its massfraction reduces (Fw value), and more compared with steam explosion stripping of acid explosion, this is also the reason that acid explosion solid content is low compared with steam explosion.In addition, because heteroproteose cell is generally short and wide, its L/W is little, therefore after its a large amount of stripping, also causes the L/W value of acid explosion pre-treatment sample slightly to improve.
Table 92# acid explosion pre-hydrolyzed solution carbohydrate components content
From the data of table 9, relative to neutral steam explosion, after acid explosion treatment, the content of polysaccharide reduces, and contents of monosaccharides increases, and monose and polysaccharide account for 31.4% and 68.6% of total reducing sugar amount respectively.With regard to monose, mainly based on pectinose and glucose, polysaccharide is then based on xylose and glucose.Acid explosion pre-treatment can make maize straw sample be in all the time among sour environment, promotes the hydrolysis of Mierocrystalline cellulose and hemicellulose in sample.Contrast two kinds of explosion treatment, the glucose content in the polysaccharide after acid explosion treatment significantly reduces.This shows, acid explosion can change into glucose monosaccharide the glucose polysaccharide of degraded, and also namely acid explosion can obtain more monose, and this is favourable to follow-up enzymolysis.
As can be seen from above-mentioned comparative study, in explosion preprocessing process, hemicellulose is degraded stripping in a large number, and content reduces, and xylogen is also degraded stripping, and sample fiber structure is destroyed, and the impact of acid vapors explosion on fibrous texture is larger.The granularity of material diminishes, and fibrous bundle is separated from each other that loose, pulp freeness increases, aperture increases, and is more conducive to the carrying out of follow-up enzyme digestion reaction.
Embodiment 4
The preparation of maize straw enzymolysis substrate:
Respectively by the pretreatment sample washes clean that example 2 and example 3 obtain, put into sealing plastics bag equilibrium water content 24h.Take neutral explosion pretreatment sample and acid explosion pretreatment sample that absolute dry mass is 10g respectively, mix than the ratio for 1:1 according to absolute dry mass, obtain the cellulose sample for follow-up enzymolysis.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. maize straw produces a pretreatment process for ethanol, it is characterized in that, comprises the following steps:
S1: get corn stalk raw material, mechanical disintegration to 3 ~ 5cm, be air-dryly in its natural state less than 5% ~ 10% to moisture, obtains maize straw powder, Air drying storage under ambient conditions, for subsequent use;
S2. prehydrolysis: by S1 step gained maize straw powder equilibrium water content, add water and acid solution, carry out slightly acidic middle pressure steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collect sample a and hydrolyzed solution respectively, for subsequent analysis;
S3. prehydrolysis: by S1 step gained maize straw powder equilibrium water content, carry out neutral steam explosion pre-treatment, after hydrolysis reaction terminates, by explosion sample and hydrolyzed solution centrifugation, collects sample b and hydrolyzed solution, respectively for subsequent analysis;
S4. the explosion sample obtained S2 and S3 carries out chemical composition analysis and morphological structure analysis, carries out sugar analysis to pre-hydrolyzed solution;
S5. collect the sample a after S2 and S3 prehydrolysis and sample b respectively, after washes clean, mix than for the ratio of 1:1 ~ 3:1 according to absolute dry mass, obtain the cellulosic substrate for follow-up enzymatic hydrolysis and fermentation.
2. maize straw produces the pretreatment process of ethanol according to claim 1, and it is characterized in that, described maize straw takes from the Northeast of China.
3. maize straw produces the pretreatment process of ethanol according to claim 2, it is characterized in that, in S2, the pretreated condition of described slightly acidic middle pressure steam explosion is: concentration of substrate is 0 ~ 20%, acid solution massfraction is 0 ~ 2%, and burstpressures is 0.8 ~ 1.0MPa, and the reaction times is 0 ~ 15min.
4. maize straw produces the pretreatment process of ethanol according to claim 3, it is characterized in that, in S3, the pretreated condition of described neutral steam explosion is: concentration of substrate is 0 ~ 20%, acid solution massfraction is 0%, and burstpressures is 0.8 ~ 1.0MPa, and the reaction times is 0 ~ 15min.
5. maize straw produces the pretreatment process of ethanol according to claim 3, and it is characterized in that, described acid solution is sulphuric acid soln.
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| CN105421129A (en) * | 2015-12-04 | 2016-03-23 | 大连工业大学 | Method for preparing nano-crystalline cellulose by taking corn stalks as raw materials and application thereof |
| CN105886554A (en) * | 2016-02-27 | 2016-08-24 | 华南理工大学 | Two-step pre-processing method for producing cellulosic ethanol from corn stalks |
| CN106832330A (en) * | 2017-01-18 | 2017-06-13 | 华南理工大学 | The technique of recovery and the purification of residual lignin after a kind of steam blasting pretreatment |
| CN110241006A (en) * | 2019-07-03 | 2019-09-17 | 上海中溶科技有限公司 | The pretreatment unit of cellulose and hemicellulose producing and ethanol is extracted from agricultural crop straw |
| CN111500658A (en) * | 2020-04-10 | 2020-08-07 | 大连海洋大学 | Method for increasing value and utilizing biomass in multiple ways |
| CN112666122A (en) * | 2020-12-30 | 2021-04-16 | 华南理工大学 | Method for rapidly detecting glucose and moisture content after corn straw blasting pretreatment |
| CN112782032A (en) * | 2020-12-30 | 2021-05-11 | 华南理工大学 | Method for quickly detecting physical property parameters of raw materials after acidic blasting pretreatment of cellulose and ethanol prepared from wood fiber raw materials and application |
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| CN105421129A (en) * | 2015-12-04 | 2016-03-23 | 大连工业大学 | Method for preparing nano-crystalline cellulose by taking corn stalks as raw materials and application thereof |
| CN105886554A (en) * | 2016-02-27 | 2016-08-24 | 华南理工大学 | Two-step pre-processing method for producing cellulosic ethanol from corn stalks |
| CN106832330A (en) * | 2017-01-18 | 2017-06-13 | 华南理工大学 | The technique of recovery and the purification of residual lignin after a kind of steam blasting pretreatment |
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| CN111500658B (en) * | 2020-04-10 | 2023-10-03 | 大连海洋大学 | Method for multi-way value-added utilization of biomass |
| CN112666122A (en) * | 2020-12-30 | 2021-04-16 | 华南理工大学 | Method for rapidly detecting glucose and moisture content after corn straw blasting pretreatment |
| CN112782032A (en) * | 2020-12-30 | 2021-05-11 | 华南理工大学 | Method for quickly detecting physical property parameters of raw materials after acidic blasting pretreatment of cellulose and ethanol prepared from wood fiber raw materials and application |
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