CN103981221A - Method for preparing ethanol through cassava chip fermentation - Google Patents
Method for preparing ethanol through cassava chip fermentation Download PDFInfo
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- CN103981221A CN103981221A CN201410233386.0A CN201410233386A CN103981221A CN 103981221 A CN103981221 A CN 103981221A CN 201410233386 A CN201410233386 A CN 201410233386A CN 103981221 A CN103981221 A CN 103981221A
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Abstract
The invention relates to a method for preparing ethanol through cassava chip fermentation. The method comprises the steps of with cassava sheets as raw materials, smashing, extruding, carrying out acid washing, separating, carrying out alkaline washing, carrying out acid washing, carrying out secondary enzymolysis, separately fermenting and concentrating to obtain ethanol. By using the method, all effective components in the cassava chips are utilized to the maximum extent, the fermentation time is shortened, and the yield of ethanol is increased.
Description
Technical field
The present invention relates to a kind of production method of utilizing cassava slice fermentative production of ethanol.
Background technology
Cassava is world's plantation one of potato class plant very widely, mainly plants status in subtropical and tropical zones.Cassava is existing also can directly be processed into food mainly for the production of tapioca (flour), can also pass through the products such as fermentative production of ethanol, sorbyl alcohol, citric acid.Cassava does large 70% left and right of middle starch content, is suitable as very much the raw materials for production of ethanol.The cassava of take has other grain class fermentative production of ethanol as fermenting raw materials production ethanol can reduce, and has obvious strategy and social benefit.
In prior art, the technique that the cassava of take is raw material production ethanol, generally adopts High Temperature High Pressure cooking process to liquefy, and can cause like this Fermentable substrate qualitative change in raw material to run off, and consumes energy higher; Secondly, in prior art, Major Enzymes hydrolysis and fermentation is to liking starch, and the Mierocrystalline cellulose in cassava slice, hemicellulose and other polymerization carbohydrate fail effectively to utilize; In addition, whole technique enzymolysis efficiency is not high, is embodied in: (1) simultaneously plurality of enzymes carries out enzymolysis, the condition suitable because of various enzymes is different, starch in cassava slice, Mierocrystalline cellulose and hemicellulose, and other polymerization carbohydrates are difficult to simultaneously complete hydrolysis and become glucose, final alcohol getting rate is not high; (2) gradation enzymolysis, although each composition hydrolysis is completely, alcohol getting rate improves, enzymolysis time extends.Therefore, further study cassava slice and produce ethanol, reduce the usage quantity of various enzymes, shorten enzymolysis time, thereby improve conversion coefficient and alcohol getting rate, for effectively utilizing cassava slice to there is important practical significance.
Summary of the invention
The object of this invention is to provide a kind of saving time and the method for the cassava slice alcohol prepared by fermenting of high alcohol getting rate.
For realizing object of the present invention, by the following technical solutions.
A method for cassava slice alcohol prepared by fermenting, the method comprises following concrete steps:
A. cassava slice is added to water infiltration, wet pulverization;
B. by the product after pulverizing, enter forcing machine extruding;
C. get the pressing materials of step b gained, add the water of 3 times of quality of cassava slice, then acid adding to be adjusted to pH be 2-6, be heated to 80-95 ℃, stir and soak 2-4h, filter to get filtrate and filter residue A, filtrate decompression be concentrated into original volume 1/3 filtrate A;
D. get the filter residue A of step c gained, add the water of 3 times of quality of cassava slice, adding alkali, to be adjusted to pH be 7-9, is heated to 80-95 ℃, stirs and soak after 2-6h, adds acid for adjusting pH to 4-7, be incubated 80-95 ℃ and stir immersion 2-4h;
E. in the material of steps d gained, add zytase and saccharifying enzyme, after the ultrasonic echography 1-2min that is 160-200W with power, close ultrasonic wave, be incubated enzymolysis after 1.5 hours, again ultrasonic echography 1-2min, insulation enzymolysis is after 1.5 hours, and hydrolysis temperature is 40-60 ℃;
F. in the material of step e gained, add saccharifying enzyme, amylase and cellulase, after the ultrasonic echography 1-2min that is 100-150W with power, close ultrasonic wave, insulation enzymolysis is after 6 hours, again after ultrasonic echography 1-2min, close ultrasonic wave, insulation enzymolysis is after 6 hours, and hydrolysis temperature is 60-80 ℃.After enzymolysis completes, filter to get filtrate and filter residue B, filtrate decompression is concentrated into original volume 1/3 and obtains liquor B;
G. in step c gained filtrate A, access the fermented liquid A containing ethanol finishing after red tree yeast fermentation;
H. in step f gained liquor B, access the fermented liquid B containing ethanol after fermentation by saccharomyces cerevisiae;
I. get after the fermented liquid A of step g and the fermented liquid B of step h filter and mix, then through rectification and purification, to obtain concentration be more than 95% ethanol.
After step a cassava slice wet pulverization, cross 20 mesh sieves, the quality that adds water is the 20-45% of cassava slice quality.Add the water yield too much unsuitable herein, soak material.
Cassava slice material after pulverizing and sieving is in forcing machine, under the parameter of setting, push, in exit instant decompression, thereby expand to obtain fluffy materials, be conducive on the one hand the separated of starch in cassava slice, Mierocrystalline cellulose and xylogen, improve starch and the accessibility of Mierocrystalline cellulose to enzyme, next is extruded with to be beneficial to breaks cellulosic crystalline texture, further improves the accessibility of Mierocrystalline cellulose to enzyme.Forcing machine described in step b is the conventional single screw extrusion machine of plastic working industry, and extrusion temperature is 70-90 ℃, screw speed 80-100 rev/min, and the filtrate A described in step b is concentrated acquisition after nanofiltration membrane is filtered, entering film pressure is 2-4Mpa.
The acid solution that step c and steps d add is one or more combination of hydrochloric acid, phosphoric acid, sulfuric acid, citric acid; The alkali lye that steps d adds is one or more combination of potassium hydroxide, sodium hydroxide and calcium hydroxide.Wherein, step c adds acid solution cleaning gained filtrate A for containing the mixing solutions of pentose and other soluble sugar; Filter residue A is starch, Mierocrystalline cellulose, hemicellulose and xylogen.Steps d first use alkali cleaning with acid for adjusting pH to acid enzymolysis, alkali cleaning improves cellulosic hydrolysis efficiency.
The add-on of step e zytase is the dry cassava slice of 1.0-1.5U/g, and the add-on of saccharifying enzyme is the dry cassava slice of 60-80U/g.This step adds 2 kinds of enzymes simultaneously, the hydrolysis of the hemicellulose existing in zytase promotion cassava slice, and saccharifying enzyme promotes the first one-step hydrolysis of starch in cassava slice.
The add-on of step f saccharifying enzyme is the dry cassava slice of 60-80U/g, and diastatic add-on is the dry cassava slice of 30-40U/g, and the add-on of cellulase is the dry cassava slice of 2-4U/g.This step adds 3 kinds of enzymes simultaneously, the collaborative hydrolysis that promotes to exist in cassava slice Mierocrystalline cellulose and starch.
Step e and step f are used ultrasonic, can accelerate the dispersion of enzyme and the contact that promotes enzyme-to-substrate, improve percent hydrolysis.Ultrasonic power is set in 160-200W and 100-150W, and the size of power is determined through preferred with using the kind of enzyme.
Step g finishes red tree yeast-inoculated concentration 5-10g/L, the aerobic condition bottom fermentation 36-48h that is 0.2-0.8 at 30-50 ℃, ventilation ratio.
Step h yeast saccharomyces cerevisiae inoculum density 20-40g/L, at 30-50 ℃, anaerobic condition bottom fermentation 36-48h.
The method of a kind of cassava slice alcohol prepared by fermenting provided by the invention, its advantage is:
(1) cassava slice, after extruding, can effectively make starch, Mierocrystalline cellulose and lignin separation, increases the accessibility of starch and Mierocrystalline cellulose and enzyme, be hydrolyzed more abundant, conversion coefficient raising.
(2) step C acid solution washing containing soluble sugars such as pentoses, and ferment separately for this kind of sugar, improve the comprehensive utilization ratio of cassava slice.
(3) enzymolysis divides secondary to carry out, add first zytase and saccharifying enzyme, be amylase, saccharifying enzyme and cellulase for the second time, the main object of secondary enzymolysis is different, object is hemicellulose first, and object is starch and Mierocrystalline cellulose for the second time, enters the secondary enzymolysis scheme that the present invention proposes, improve hydrolysis efficiency, can make full use of the effective constituent in cassava slice.
(4) in enzymolysis process, use ultrasonic power, can increase on the one hand the contact of enzyme-to-substrate, improve on the other hand the activity of enzyme under acidic conditions, improve percent hydrolysis, reduce hydrolysis time.
Embodiment
Below in conjunction with several embodiment, further illustrate the present invention and innovation.Should be appreciated that listed embodiment is only for illustrating the present invention but not limitation of the invention further, those skilled in the art can suitably adjust embodiment after fully understanding, these are still within protection scope of the present invention.
embodiment 1
10kg cassava slice is added to 2.0kg water, after pulverizing, cross 20 mesh sieves, under 70 ° of C, 80 revs/min of conditions of screw speed, through screw rod, make pressure, in the expanded porous fluffy materials that obtains of exit instant decompression; By adding 20kg water in above-mentioned porous fluffy materials, under agitation condition, with the vitriol oil, regulate pH2.0, be heated to 80 ℃, stir and soak 2.0h, filter to get filtrate and filter residue A, filtrate decompression is concentrated into original volume 1/3 and obtains filtrate A;
Under the aerobic condition that is 0. 2 at 30 ° of C, ventilation ratio by filtrate A, after finishing red trunk yeast fermentation 36h, 5 g/L obtain ethanolic soln;
In filter residue A, add 20kg water, under agitation condition, with sodium hydroxide, regulating pH is 7.0, is heated to 80 ℃, stir and soak 2.0h, adding sulphur acid for adjusting pH is 4.0, after heat-insulation soaking 2h, add zytase and Glucoamylase hydrolysis, add-on is the dry cassava slice of zytase 1.0U/g, the dry cassava slice of saccharifying enzyme 60U/g, then close ultrasonic wave after the ultrasonic echography 1min that is 160W with power, insulation enzymolysis is after 1.5 hours, ultrasonic echography 1min, was incubated enzymolysis after 1.5 hours again, and hydrolysis temperature is 40 ℃;
In the material of above-mentioned gained, add saccharifying enzyme, amylase and cellulase, the add-on of saccharifying enzyme is the dry cassava slice of 60U/g, and diastatic add-on is the dry cassava slice of 30U/g, and the add-on of cellulase is the dry cassava slice of 2U/g.After the ultrasonic echography 2min that is 100W with power, close ultrasonic wave, insulation enzymolysis, after 6 hours, is closed ultrasonic wave after ultrasonic echography 2min again, and insulation enzymolysis is after 6 hours, and hydrolysis temperature is 60 ℃.After enzymolysis completes, filter to get filtrate and filter residue B, filtrate decompression is concentrated into original volume 1/3 and obtains liquor B;
Liquor B is obtained to ethanolic soln under 30 ° of C, anaerobic fermentation conditions after 20 g/L fermentation by saccharomyces cerevisiae 36h.
After the ethanolic soln rectifying the concentrate finally fermentation of filtrate A and liquor B being obtained, obtain the ethanol that purity is 95 %.
embodiment 2
10kg cassava slice is added to 2.5kg water, after pulverizing, cross 20 mesh sieves, under 80 ° of C, 95 revs/min of conditions of screw speed, through screw rod, make pressure, in the expanded porous fluffy materials that obtains of exit instant decompression; To in above-mentioned porous fluffy materials, add 20kg water, be 5.4 with phosphorus acid for adjusting pH under agitation condition, is heated to 90 ℃, stirs and soak 3h, filters to get filtrate and filter residue A, and filtrate decompression is concentrated into original volume 1/3 and obtains filtrate A;
Under the aerobic condition that is 0.6 at 45 ° of C, ventilation ratio by filtrate A, after finishing red trunk yeast fermentation 36h, 8 g/L obtain ethanolic soln;
In filter residue A, add 20kg water, under agitation condition, with sodium hydroxide, regulating pH is 8.0, is heated to 90 ℃, stir and soak 3.5h, the acid for adjusting pH that phosphorates is 5.5, after heat-insulation soaking 2h, add zytase and Glucoamylase hydrolysis, add-on is the dry cassava slice of zytase 1.3U/g, the dry cassava slice of saccharifying enzyme 70U/g, then close ultrasonic wave after the ultrasonic echography 1min that is 180W with power, insulation enzymolysis is after 1.5 hours, ultrasonic echography 1min, was incubated enzymolysis after 1.5 hours again, and hydrolysis temperature is 50 ℃;
In the material of above-mentioned gained, add saccharifying enzyme, amylase and cellulase, the add-on of saccharifying enzyme is the dry cassava slice of 70U/g, and diastatic add-on is the dry cassava slice of 35U/g, and the add-on of cellulase is the dry cassava slice of 3U/g.After the ultrasonic echography 1min that is 120W with power, close ultrasonic wave, insulation enzymolysis, after 6 hours, is closed ultrasonic wave after ultrasonic echography 1min again, and insulation enzymolysis is after 6 hours, and hydrolysis temperature is 70 ℃.After enzymolysis completes, filter to get filtrate and filter residue B, filtrate decompression is concentrated into original volume 1/3 and obtains liquor B;
Liquor B is obtained to ethanolic soln under 45 ° of C, anaerobic fermentation conditions after 30 g/L fermentation by saccharomyces cerevisiae 36h.
After the ethanolic soln rectifying the concentrate finally fermentation of filtrate A and liquor B being obtained, obtain the ethanol that purity is 95 %.
embodiment 3
10kg cassava slice is added to 4.5kg water, after pulverizing, cross 20 mesh sieves, under 90 ° of C, 100 revs/min of conditions of screw speed, through screw rod, make pressure, in the expanded porous fluffy materials that obtains of exit instant decompression; To in above-mentioned porous fluffy materials, add 20kg water, be 6.0 with phosphorus acid for adjusting pH under agitation condition, is heated to 95 ℃, stirs and soak 3h, filters to get filtrate and filter residue A, and filtrate decompression is concentrated into original volume 1/3 and obtains filtrate A;
Under the aerobic condition that is 0.8 at 50 ° of C, ventilation ratio by filtrate A, after finishing red trunk yeast fermentation 36h, 10 g/L obtain ethanolic soln;
In filter residue A, add 20kg water, under agitation condition, with sodium hydroxide, regulating pH is 9.0, is heated to 95 ℃, stir and soak 6.0h, the acid for adjusting pH that phosphorates is 7.0, after heat-insulation soaking 4h, add zytase and Glucoamylase hydrolysis, add-on is the dry cassava slice of zytase 1.5U/g, the dry cassava slice of saccharifying enzyme 80U/g, then close ultrasonic wave after the ultrasonic echography 2min that is 200W with power, insulation enzymolysis is after 1.5 hours, ultrasonic echography 2min, was incubated enzymolysis after 1.5 hours again, and hydrolysis temperature is 60 ℃;
In the material of above-mentioned gained, add saccharifying enzyme, amylase and cellulase, the add-on of saccharifying enzyme is the dry cassava slice of 80U/g, and diastatic add-on is the dry cassava slice of 40U/g, and the add-on of cellulase is the dry cassava slice of 4U/g.After the ultrasonic echography 2min that is 150W with power, close ultrasonic wave, insulation enzymolysis, after 6 hours, is closed ultrasonic wave after ultrasonic echography 2min again, and insulation enzymolysis is after 6 hours, and hydrolysis temperature is 80 ℃.After enzymolysis completes, filter to get filtrate and filter residue B, filtrate decompression is concentrated into original volume 1/3 and obtains liquor B;
Liquor B is obtained to ethanolic soln under 50 ° of C, anaerobic fermentation conditions after 40g/L fermentation by saccharomyces cerevisiae 48h.
After the ethanolic soln rectifying the concentrate finally fermentation of filtrate A and liquor B being obtained, obtain the ethanol that purity is 95 %.
comparative example 1
After cassava slice wet pulverization, without forcing machine, process, all the other press the method alcohol prepared by fermenting of embodiment 2..
comparative example 2
Press the method alcohol prepared by fermenting of embodiment 2, wherein ultrasonic wave is used not ultrasonic during enzymolysis..
comparative example 3
The method alcohol prepared by fermenting of pressing embodiment 2, enzymolysis carries out simultaneously, and the add-on of enzyme is consistent with embodiment 2, and hydrolysis temperature is 60 ℃, enzymolysis time 16h..
comparative example 4
10kg cassava slice is added to 2.5kg water, after pulverizing, cross 20 mesh sieves, under 80 ° of C, 95 revs/min of conditions of screw speed, through screw rod, make pressure, in the expanded porous fluffy materials that obtains of exit instant decompression; To in above-mentioned porous fluffy materials, add 60kg water, under agitation condition, with sodium hydroxide, regulating pH is 8.0, is heated to 95 ℃, stirs and soaks 3.5h, and the acid for adjusting pH that phosphorates is 5.5, and after heat-insulation soaking 3h, all the other are undertaken by the method for embodiment 2.
embodiment 4
Ethanol content is measured: press GB/T 678-2002 ethanol content measuring method and measure.
Alcohol yied=ethanol weight/cassava slice weight * 100%.Embodiment 1-3, comparative example 1-4 alcohol yied the results are shown in Table 1, and result shows, the present invention program's alcohol getting rate is higher, reduce extruding, do not use ultrasonic, change mode of action, not separate fermentation, alcohol getting rate is decline to some extent all.
Table 1 embodiment and comparative example's alcohol getting rate result
| Group | Alcohol yied (%) |
| Embodiment 1 | 55.3 |
| Embodiment 2 | 56.1 |
| Embodiment 3 | 55.8 |
| Comparative example 1 | 51.4 |
| Comparative example 2 | 50.6 |
| Comparative example 3 | 50.9 |
| Comparative example 4 | 49.7 |
Claims (9)
1. a method for cassava slice alcohol prepared by fermenting, the method comprises:
A. cassava slice is added to water infiltration, wet pulverization;
B. by the product after pulverizing, enter forcing machine extruding;
C. get the pressing materials of step b gained, add the water of 3 times of quality of cassava slice, then acid adding to be adjusted to pH be 2-6, be heated to 80-95 ℃, stir and soak 2-4h, filter to get filtrate and filter residue A, filtrate decompression be concentrated into original volume 1/3 filtrate A;
D. get the filter residue A of step c gained, add the water of 3 times of quality of cassava slice, adding alkali, to be adjusted to pH be 7-9, is heated to 80-95 ℃, stirs and soak after 2-6h, adds acid for adjusting pH to 4-7, be incubated 80-95 ℃ and stir immersion 2-4h;
E. in the material of steps d gained, add zytase and saccharifying enzyme, after the ultrasonic echography 1-2min that is 160-200W, close with power, insulation enzymolysis is after 1.5 hours, and ultrasonic 1-2min, was incubated enzymolysis after 1.5 hours again, and hydrolysis temperature is 40-60 ℃;
F. in the material of step e gained, add saccharifying enzyme, amylase and cellulase, after the ultrasonic echography 1-2min that is 100-150W with power, close, insulation enzymolysis, after 6 hours, is closed after ultrasonic 1-2min again, insulation enzymolysis is after 6 hours, and hydrolysis temperature is 60-80 ℃;
After enzymolysis completes, filter to get filtrate and filter residue B, filtrate decompression is concentrated into original volume 1/3 and obtains liquor B;
G. in step c gained filtrate A, access the fermented liquid A containing ethanol finishing after red tree yeast fermentation;
H. in step f gained liquor B, access the fermented liquid B containing ethanol after fermentation by saccharomyces cerevisiae;
I. get after the fermented liquid A of step g and the fermented liquid B of step h filter and mix, then through rectification and purification, to obtain concentration be more than 95% ethanol.
2. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that crossing 20 mesh sieves after step a cassava slice wet pulverization, and the quality that adds water is the 20-45% of cassava slice quality.
3. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that the forcing machine described in step b is conventional single screw rod or the twin screw extruder of plastic working industry, and extrusion temperature is 70-90 ℃, screw speed 80-100 rev/min.
4. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that acid solution that step c and steps d add is one or more combination of hydrochloric acid, phosphoric acid, sulfuric acid, citric acid; The alkali lye that steps d adds is one or more combination of potassium hydroxide, sodium hydroxide and calcium hydroxide.
5. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, the add-on that it is characterized in that step e zytase is the dry cassava slice of 1.0-1.5U/g, the add-on of saccharifying enzyme is the dry cassava slice of 60-80U/g.
6. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, the add-on that it is characterized in that step f saccharifying enzyme is the dry cassava slice of 60-80U/g, diastatic add-on is the dry cassava slice of 30-40U/g, and the add-on of cellulase is the dry cassava slice of 2-4U/g.
7. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that the filtrate A described in step b is concentrated acquisition after nanofiltration membrane is filtered, and entering film pressure is 2-4Mpa; Liquor B described in step f is concentrated acquisition after nanofiltration membrane is filtered, and entering film pressure is 2-4Mpa.
8. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that step g finishes red tree yeast-inoculated concentration 5-10g/L, the aerobic condition bottom fermentation 36-48h that is 0.2-0.8 at 30-50 ℃, ventilation ratio.
9. the method for a kind of cassava slice alcohol prepared by fermenting according to claim 1, is characterized in that step h yeast saccharomyces cerevisiae inoculum density 20-40g/L, at 30-50 ℃, anaerobic condition bottom fermentation 36-48h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463032A (en) * | 2015-12-14 | 2016-04-06 | 山西大同大学 | Pretreatment method for raw material cassava of fuel ethanol |
| CN105463032B (en) * | 2015-12-14 | 2019-01-18 | 山西大同大学 | A kind of preprocess method of fuel ethyl hydrate raw material cassava |
| CN112708640A (en) * | 2021-01-21 | 2021-04-27 | 广东莞垄农业生态科技有限公司 | Method for extracting alcohol by processing and fermenting cassava extracted starch |
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