CN104109694B - A kind of method of sweet sorghum stalk comprehensive utilization - Google Patents
A kind of method of sweet sorghum stalk comprehensive utilization Download PDFInfo
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- CN104109694B CN104109694B CN201310660654.2A CN201310660654A CN104109694B CN 104109694 B CN104109694 B CN 104109694B CN 201310660654 A CN201310660654 A CN 201310660654A CN 104109694 B CN104109694 B CN 104109694B
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Abstract
The present invention provides a kind of method of sweet sorghum stalk comprehensive utilization.It is after crushing fresh and sweet broomcorn straw defoliation, to be ground into slurry, add extractant, extract tannin；Then pectin, ethyl alcohol, cellulose and lignin are prepared again, so that sweet sorghum stalk be made adequately to be used.The present invention realizes sweet sorghum stalk processing environment close friend and intensive efficient target, takes full advantage of the utility in sweet sorghum stalk, increases sweet sorghum stalk processing added value, improves the level of resources utilization, realize production process zero release of pollutant.Be conducive to improve the enthusiasm of Cotton Varieties by Small Farming Households sugar grass, and the raw material site of sugar grass will effectively be promoted to build.
Description
Technical field
The invention belongs to biological materials and energy technology field, specifically, being related to a kind of comprehensive benefit of sweet sorghum stalk
Method.
Background technique
Sugar grass is one of highest crops of biological yield, there is long cultivation history, south and the north in China
There is large area plantation.Fresh sweet sorghum stalk dry matter about containing cellulose 20~22%, lignin 10~12%, hemicellulose
Element 16~19%, pectin 10~13%, crude protein 3~4%, total sugar content 35~41%, tannin 0.4~2.5%, crude fat,
Minerals etc. other 3~5%.
Currently, sweet sorghum stalk utilizes mainly for the preparation of ethyl alcohol, through pilot scale business accounting, high expensive, benefit is relatively low,
It always can not industrialization promotion application.The comprehensive utilization of existing sweet sorghum stalk is at most " ethyl alcohol-cardboard ", " ethyl alcohol-vinasse
Feed ", " ethyl alcohol-xylose " coproduction are also not thorough the utilization of sweet sorghum stalk utility, and economic benefit fails sufficiently to send out
It waves；Such as, for paperboard fibres obtained only up to the level of production cardboard or carton, the added value of lees feeds is lower, even
Xylose is extracted, economic benefit is also up for improving.In this way, not only resulting in waste of resources, but also a large amount of discharges are generated, cost of material obtains not
To raising, the enthusiasm of Cotton Varieties by Small Farming Households sugar grass is seriously affected, the scale in sugar grass raw material base can not expand development, thus
Constrain fuel ethanol industrial development.
Sugar grass is the plant few in number higher C4 crop containing tannin.Tannin is also known as tannin extract, in medicine, printing and dyeing, changes
The industries such as work, platform gold, wine brewing, stationery are widely applied.Traditional tannin production is extracted from green persimmon and Chinese gall, every production
10000 tons of tannin takes around 100,000 mu of persimmon or Gallnut forest cultivated area.Since land resource is limited, traditional tannin
Extracting method is unable to satisfy the market demand.Had in recent years using pine needle and the extraction of some wild plants, but still is unable to satisfy market
Demand.As can extracting tannin using sweet sorghum stalk, it can both increase the added value of sweet sorghum stalk processing, tannin city can also be supplemented
Field is insufficient.In addition, ethyl alcohol, pectin, fiber, lignin, feed are China's goods and materials in short supply." 12th Five-Year Plan " plans that China promotes combustion
5,000,000 tons of ethyl alcohol of material, existing production capacity is less than 3,000,000 tons.Pectin, fiber and lignin rely on import for a long time in the past 10 years and meet state
The interior market demand.Though China is large agricultural country, food supply is very nervous and feed lacks country, and protein feed especially lacks
It is weary.Domestic demand is pulled with this, a large amount of above goods and materials productions in short supply of development, the exactly good opportunity of sweet sorghum stalk processing industry development.
Therefore, sweet sorghum stalk whole body is all precious.Sweet sorghum stalk useful component is sufficiently extracted, not only its economic value will be at
Several times increase, promoted sweet sorghum stalk cost of material, improve Cotton Varieties by Small Farming Households sugar grass enthusiasm, drive sugar grass planting industry and
Related processing industry sustainable development, and fuel ethanol industrialization development is promoted, meanwhile, it avoids the wasting of resources and largely gives up
Object discharge.
Summary of the invention
Place in order to overcome the deficiencies of the prior art, the present invention provide a kind of method of sweet sorghum stalk comprehensive utilization, joint
Ethyl alcohol, tannin, pectin, fiber, lignin are produced, to reduce the comprehensive utilization cost of sweet sorghum stalk, increases sugar grass straw
Stalk processes added value, improves the level of resources utilization, realizes production process zero release of pollutant.
The technical solution adopted by the present invention to solve the technical problems is that the method for sweet sorghum stalk comprehensive utilization includes
Following steps:
(1) it prepares stalk slurry: fresh and sweet broomcorn straw being removed into leaf, after crushing, is milled into the sugar grass of 80 mesh or more
Stalk slurry；
(2) extraction prepares tannin: sweet sorghum stalk slurry is put into fractionating column, extractant is added, it is quiet after being sufficiently stirred
Set layering；Upper layer of extraction liquid is pumped into distiller, extractant is distilled to recover and tannin is made after extractant evaporation；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, sweet sorghum stalk slurry of squeezing out
Syrup, then after the sweet sorghum stalk slurry slag after squeezing is impregnated with clear water, carry out twice pressing, and the sugar that will be squeezed out twice
Juice mixing for standby use；
(4) it prepares pectin: the sweet sorghum stalk slurry slag after twice pressing being put into reactor tank, and dilute sulfuric acid is added；
Then lead to and be steam heated to 80~100 DEG C, and keep the temperature 20~40min, make the pectin dissolved well in sweet sorghum stalk slurry slag,
It is squeezed again, separates pectin solution with sweet sorghum stalk slurry slag；Active carbon is added in the pectin solution squeezed out, it is right
Ethyl alcohol is added in liquid pectin, pectin is precipitated for pectin solution decoloration, the liquid pectin obtained after filtering；Then de- with centrifuge
Except solution, pectin is extracted；Pectin is cleaned, dry, pulverize, and pectin finished product is made；The solution isolated is pumped into distiller, is returned
Receive ethyl alcohol；Remaining acid solution is used for subsequent pressurization acidolysis solution；
(5) it prepares ethyl alcohol: the sweet sorghum stalk slurry slag after pectin solution will be squeezed in step (4) and remaining acid solution is mixed
It closes uniformly, and the sulfuric acid concentration of mixed material is adjusted to 3~8 ‰, be pumped into reactor tank, be passed through and be steam heated to 115~125
DEG C, 50~90min is kept, pressurization acid hemolysis process is completed, makes hemicellulose fully degraded in acid solution, then leading to cold water makes to react
Tank is cooled to 100 DEG C hereinafter, syrup of squeezing out；The syrup squeezed out is mixed with the syrup that step (3) is squeezed, sugar upon mixing
Ammonium hydroxide is added in juice, makes (NH in half congealed juice4)2SO4Content be 1~1.5g/L；Nutritive salt is added, white lime is then added, it will
The pH value of syrup is adjusted to 4~5；
1/1100~1/900 of syrup quality after modulating is taken, the sugar aqueous solution that pol is 2% is diluted to, puts into yeast tank
In, then put into the saccharic alcohol Angel Yeast and candida utili of modulated syrup quality 2/11000~2/9000, saccharic
Alcohol Angel Yeast and candida utili are mixed in the ratio of 5~8:2~5, and are increased with sterile wind to liquid glucose dilute in yeast tank
Oxygen carries out yeast and expands numerous, the numerous end of 100~150min expansion；
The yeast juice of modulated syrup and expansion after numerous is sent into fermentation bag, fermentation bag is then closed and carries out anaerobic fermentation 30
~48h detects residual reducing sugar content, and less than 0.5%, alcoholic fermentation terminates content of reducing sugar；By the wine liquid after fermenting-ripening,
It is sent into distillation still, thick wine, then rectifying, dehydration is extracted by distillation, alcohol fuel is made；The viable yeast of retained sediments in fermentation bag
Mud, for next liquid glucose fermentation, after reusing 5~6 times, yeast activity decline is recycled yeast, is cleaned, dry, prepares yeast
Protein feed；
(6) prepare cellulose and lignin: the sweet sorghum stalk slurry slag after squeezing syrup in step (5) is soaked through clear water
After bubble, dilute syrup is squeezed out；To squeeze out that the sweet sorghum stalk slurry slag after dilute syrup puts into 4~6 times of material residue quality 30%
In ethyl alcohol, and KOH is added as catalyst, after mixing, is sent into enamel reactor, it is closed, it is passed through steam heating, makes temperature
Degree rises to 95~105 DEG C, keeps 55~65min, completes the pressurization alcoholysis process of slag charge, drop the lignin of slag charge sufficiently
Solution；Then, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；Cellulose
Slag charge is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, and cellulose is made in bleaching；Lignin liquor is distilled, is recycled
Wine liquid；Lignin filtering will be precipitated, lignin is made in cleaning, drying；Recycling wine liquid continues on for alcohol analysis, or for distilling combustion
Expect ethyl alcohol.
In above-mentioned steps (1), when processing sweet sorghum stalk slurry, extractant is sent together with smashed sweet sorghum stalk
Enter in fiberizer, keeps the mixing of extractant and sweet sorghum stalk slurry more abundant.
The extractant being added in above-mentioned steps (2) is ethers；The mass ratio of sweet sorghum stalk slurry and extractant is 1:0.7
~1.1.
In above-mentioned steps (3), the mass ratio of sweet sorghum stalk slurry slag and clear water after squeezing is 1:1~1.5.
Dilute sulfuric acid concentration in above-mentioned steps (4) is 3~8 ‰, and the mass ratio of sweet sorghum stalk slurry slag and dilute sulfuric acid is
1:2.04~3.84；The mass ratio of pectin solution dry matter and active carbon is 1:0.05~0.08；The concentration of ethyl alcohol is 95%, fruit
The mass ratio of glue and ethyl alcohol is 1:0.7~1.5.
The activated carbon slag obtained after liquid pectin will be filtered out in step (4), wine liquid is distilled out slightly after drinking with step (5)
Obtained mash merges, and prepares liquid fertilizer.
Nutritive salt is MgSO in above-mentioned steps (5)4、KH2PO4And CaCl2；In the syrup that every rising tune makes, MgSO4、
KH2PO4And CaCl2Additional amount be respectively 8~12g, 4~6g and 4~6g.
The syrup squeezed in above-mentioned steps (5), or pass through decoloration, ion exchange, nanofiltration, condensing crystallizing process,
Extract the higher xylose of added value；This is because the syrup main component squeezed out is xylose, in addition also contain arabinose, gala
Sugar, mannose.
KOH in above-mentioned steps (6) as catalyst, with the sweet sorghum stalk for squeezing out addition 3O% ethyl alcohol after dilute syrup
Stock quality ratio is 1:900~1100.
Cellulose obtained in above-mentioned steps (6), using cellulose degraded, then ferments, and produces cellulosic ethanol.
Dilute sulfuric acid is replaced in the dilute syrup squeezed out in above-mentioned steps (6), or the step of being used for next batch (4), sweet tea is high
The mass ratio of fine strain of millet straw pulp material residue and dilute syrup is 1:4~6.
The method of sweet sorghum stalk of the present invention comprehensive utilization, make tannin in stalk, pectin, ethyl alcohol, fiber and
Lignin has obtained fully utilizing, and has recycled yeast, compares compared with sweet sorghum stalk processing technology, there is following advantage:
Compared with existing " solid fermentation method ", " juicing fermentation method ", the present invention is not merely with the grape of sweet sorghum stalk
Sugar, fructose, sucrose, also use xylose, the mannose fermenting alcohol of hemicellulose degradation, and alcohol yied increases substantially.
Compared with existing " beating method ", the present invention is integrated on the basis of inheriting and developing " beating method " superiority
" abstraction technique ", " acidolysis technology " and " alcoholysis technology " further excavates the utility value of sweet sorghum stalk resource, sufficiently extracts
The useful component of sweet sorghum stalk makes sweet sorghum stalk development and utilization from refining ethyl alcohol single product, it is a variety of to be changed into exploitation
The economic benefit of the stalks deep processing such as sugar grass is greatly improved in product.
Compared with existing " ethyl alcohol-cardboard ", " ethyl alcohol-lees feeds ", " ethyl alcohol-xylose " comprehensive use, the present invention
On the basis of integrating multinomial technology, tannin, ethyl alcohol, pectin, fiber, lignin are extracted from sweet sorghum stalk, and recycle
The multiple products such as yeast.Meanwhile the present invention has fully considered the unification of sweet sorghum stalk processing and ecological environmental protection, is producing
The medicament and solvent that can be converted into fertilizer have been used in the process, have accomplished that all waste liquids, waste residue are converted into fertilizer.
Therefore, the present invention realizes sweet sorghum stalk processing environment close friend and intensive efficient target, takes full advantage of sweet tea
Utility in broomcorn straw increases sweet sorghum stalk processing added value, improves the level of resources utilization, realize production
Process contaminant zero-emission.Be conducive to improve the enthusiasm of Cotton Varieties by Small Farming Households sugar grass, and the raw material that will effectively promote sugar grass
Construction of base.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Embodiment 1:
(1) it prepares stalk slurry: after the fresh sweet sorghum straw defoliation of acquisition, being sent into pulverizer and be ground into pipe tobacco shape
Sweet sorghum stalk silk, take 1000 kilograms of stalk silks, measure its moisture content be 75%, i.e., dry matter content be 25%；Dry
In matter Soluble adhesion molecule be 48%, about 120 kilograms；Other slag charges account for 52%, and about 130 kilograms；Again by sweet sorghum stalk silk
It is sent into fiberizer and is pumped into 1100 kilograms of propyl ether simultaneously, be ground into the sweet sorghum stalk mixed slurry of 100 mesh；
(2) extraction prepares tannin: sweet sorghum stalk mixed slurry being put into fractionating column, stirs 20min, then stand
After 60min, extract liquor and slurry are sufficiently layered, the extract liquor on fractionating tank top is pumped into distiller, recycles extractant, obtained thick
2.3 kilograms of tannin；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, sweet sorghum stalk slurry of squeezing out
260 kilograms of 740 kilograms of syrup and sweet sorghum stalk slurry slag, then the sweet sorghum stalk slurry slag after squeezing is clear with 260 kilograms
After water impregnates, twice pressing, 275 kilograms of the syrup for sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slag 245,000 are carried out
Gram, and the syrup squeezed out twice is mixed, 1015 kilograms of syrups are obtained, it is spare；
(4) it prepares pectin: by the sweet sorghum stalk slurry slag after twice pressing, being put into enamel reactor, and be added
The dilute sulfuric acid that 500L concentration is 0.8%；Then lead to and be steam heated to 100 DEG C, and keep the temperature 20min, make sweet sorghum stalk slurry slag
In pectin dissolved well, then squeezed, separate pectin solution with sweet sorghum stalk slurry slag, the pectin for obtaining 450L is molten
Liquid and 210 kilograms of sweet sorghum stalk slurry slag；3040g active carbon is added in the pectin solution squeezed out, to pectin solution
Decoloration, the liquid pectin obtained after filtering are added 675L, the ethyl alcohol that concentration is 95% in liquid pectin, pectin are precipitated；Then it uses
Centrifuge removes solution, extracts pectin；Pectin is cleaned, dry, pulverize, and 38 kilograms of pectin finished products are made；It is molten by what is isolated
Liquid pump enters distiller, recycles 75% ethyl alcohol 850L；Remaining acid solution 270L is used for subsequent pressurization acidolysis solution；
(5) it prepares ethyl alcohol: 210 kilograms of the sweet sorghum stalk slurry slag after pectin solution and residual will be squeezed in step (4)
Acid solution (270L) be uniformly mixed, and the sulfuric acid concentration of mixed material is adjusted to 8 ‰, is pumped into reactor tank, be passed through steam heating
To 125 DEG C, 50min is kept, pressurization acid hemolysis process is completed, is substantially soluble in hemicellulose in acid solution, then leading to cold water makes to react
Tank is cooled to 100 DEG C hereinafter, the syrup 320L that squeezes out, and 176 kilograms of slag charge；The syrup that the syrup squeezed out and step (3) are squeezed
It mixes, ammonium hydroxide is added in syrup upon mixing, makes (NH in half congealed juice4)2SO4Content be 1.5g/L；It adds as nutritive salt
MgSO4、KH2PO4And CaCl2, respectively 11850g, 5900g and 5900g；Then white lime is added, by the pH value tune of syrup
To 5；The syrup 1335L modulated；
1/900 modulated syrup 14.83L is taken, the sugar aqueous solution that pol is 2% is diluted with water into, is put into yeast tank,
240 grams of yeast of modulated syrup quality 2/11000 are put into again, wherein saccharic alcohol Angel Yeast and candida utili point
Wei not be 192 grams and 48 grams, and carried out yeast to liquid glucose oxygenation dilute in tank with sterile wind and expand numerous, the numerous end of about 150min expansion；
The yeast juice of modulated syrup and expansion after numerous is sent into fermentation bag, fermentation bag is then closed and carries out anaerobic fermentation
48h detects residual reducing sugar content, and less than 0.5%, alcoholic fermentation terminates；By the wine liquid after fermenting-ripening, it is sent into distillation still,
40% (v/v) thick wine is extracted by distillation, then 72 kilograms of alcohol fuel of 99.2% (v/v) are extracted in rectifying, dehydration；Recycling fermentation
97 kilograms of viable yeast mud of retained sediments in bag, for the fermentation of next batch liquid glucose (after recycling 6 times, under yeast activity
Drop recycles yeast, cleans, dry, for making dry ferment protein feed)；
(6) prepare cellulose and lignin: 176 kilograms of sweet sorghum stalk slurry slag after squeezing syrup in step (5) is put
After the clear water immersion for entering 100L, dilute syrup is squeezed out；The sweet sorghum stalk slurry slag after dilute syrup will be squeezed out and put into material residue matter
In 30% ethyl alcohol of 5 times of amount, and 978 grams of KOH are added as catalyst, after mixing, are sent into enamel reactor, are passed through steaming
Vapour heating, makes temperature rise to 105 DEG C, keeps 55min, completes the pressurization alcoholysis process of slag charge, keep the lignin of slag charge abundant
Degradation；Then, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；Fiber
Plain slag charge is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, and 63 kilograms of cellulose is made in bleaching；Lignin liquor is carried out
Wine liquid is recycled in distillation；Lignin filtering will be precipitated, 25 kilograms of lignin is made in cleaning, drying；The wine liquid of recycling is for next
The alcohol of production batch is analysed, or is used for distillate fuel ethyl alcohol；
(7) it prepares liquid fertilizer: the activated carbon slag obtained after liquid pectin will be filtered out in step (4), and it is right in step (5)
Wine liquid distills out the mash slightly obtained after drinking and merges, and by pH value adjustment to 7, obtains 432 kilograms of liquid fertilizer.
2.3 kilograms of thick tannin, 38 kilograms of pectin, 63 kilograms of cellulose, 25 kilograms of lignin, ethyl alcohol is made in the present embodiment
72 kilograms and 432 kilograms of liquid fertilizer, recycle 97 kilograms of viable yeast mud.It is calculated, processes 1 ton of fresh and sweet broomcorn straw, can get
2642 yuan of profits.
Embodiment 2:
(1) it prepares stalk slurry: after the fresh sweet sorghum straw defoliation of acquisition, being sent into pulverizer and be ground into pipe tobacco shape
Sweet sorghum stalk silk；1000 kilograms of sweet sorghum stalk silk is taken to be sent into the sweet sorghum stalk that paste mill grinding machine is ground into 100 mesh
Slurry；
(2) extraction prepares tannin: sweet sorghum stalk slurry being put into fractionating column, the allyl ethyl ether that 900L is added is made
For extractant, 10min is stirred, then stands 30min, after extract liquor is sufficiently layered with slurry, the extract liquor on fractionating tank top is taken out
Enter distiller, recycles extractant, obtain 2.1 kilograms of thick tannin；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, sweet sorghum stalk slurry of squeezing out
265 kilograms of 735 kilograms of syrup and sweet sorghum stalk slurry slag, then the sweet sorghum stalk slurry slag after squeezing is clear with 300 kilograms
After water impregnates, twice pressing, 320 kilograms of the syrup for sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slag 260,000 are carried out
Gram, and the syrup squeezed out twice is mixed, 1055 kilograms of syrups are obtained, it is spare；
(4) it prepares pectin: by the sweet sorghum stalk slurry slag after twice pressing, being put into enamel reactor, and be added
The dilute sulfuric acid that 1000L concentration is 5%；Then lead to and be steam heated to 90 DEG C, and keep the temperature 30min, make in sweet sorghum stalk slurry slag
Pectin dissolved well, then squeezed, separate pectin solution with sweet sorghum stalk slurry slag, obtain the pectin solution of 810L
With 215 kilograms of sweet sorghum stalk slurry slag；2535g active carbon is added in the pectin solution squeezed out, it is de- to pectin solution
The ethyl alcohol that 891L concentration is 95% is added in liquid pectin, pectin is precipitated for color, the liquid pectin obtained after filtering；Then with from
Scheming removes solution, extracts pectin；Pectin is cleaned, dry, pulverize, and 39 kilograms of pectin finished products are made；The solution that will be isolated
It is pumped into distiller, recycles 75% ethyl alcohol 1131L；Remaining acid solution 570L is used for subsequent pressurization acidolysis solution；
(5) it prepares ethyl alcohol: 215 kilograms of the sweet sorghum stalk slurry slag after pectin solution and residual will be squeezed in step (4)
Acid solution 570L be uniformly mixed, and the sulfuric acid concentration of mixed material is adjusted to 5 ‰, is pumped into reactor tank, is passed through and is steam heated to
120 DEG C, 70min is kept, pressurization acid hemolysis process is completed, is substantially soluble in hemicellulose in acid solution, then leading to cold water makes reactor tank
100 DEG C are cooled to hereinafter, the syrup 530L that squeezes out；The syrup squeezed out is mixed with the syrup that step (3) is squeezed, upon mixing
Ammonium hydroxide is added in syrup, makes (NH in half congealed juice4)2SO4Content be 1.25g/L；Add the MgSO as nutritive salt4、KH2PO4
And CaCl2, respectively 15850g, 7900g and 7900g；Then white lime is added, the pH value of syrup is adjusted to 4.5；It is adjusted
The syrup 1585L made；
1/1000 syrup adjusted is taken, sugared concentration is adjusted to 2%；Add 288 grams of yeast of syrup 2/10000 after modulating,
Wherein, Angel Yeast and Candida utilis bacterium are respectively 144 grams and 144 grams.And saccharomycete oxygenation is given with sterile wind, carry out yeast expansion
Numerous, 120min expands numerous end.
By expand it is numerous after yeast and after modulated syrup is sufficiently mixed, be sent into fermentation bag, then close fermentation bag and carry out
Anaerobic fermentation 39h detects residual reducing sugar content, and less than 0.5%, alcoholic fermentation terminates content of reducing sugar；After fermenting-ripening
Wine liquid, be sent into distillation still, by distillation extract 40% (v/v) thick wine, then rectifying, dehydration extract 99.2% (v/v) fuel
72 kilograms of ethyl alcohol；107 kilograms of viable yeast mud for recycling retained sediments in fermentation bag ferment for next batch liquid glucose；
(6) prepare cellulose and lignin: 180 kilograms of sweet sorghum stalk slurry slag after squeezing syrup in step (5) is put
After the clear water immersion for entering 100L, dilute syrup is squeezed out；The sweet sorghum stalk slurry slag after dilute syrup will be squeezed out and put into material residue matter
In 30% ethyl alcohol of 5 times of amount, and 900 grams of KOH are added as catalyst, after mixing, are sent into enamel reactor, are passed through steaming
Vapour heating, makes temperature rise to 100 DEG C, keeps 60min, completes the pressurization alcoholysis process of slag charge, keep the lignin of slag charge abundant
Degradation；Then, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；Fiber
Plain slag charge is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, and 65 kilograms of cellulose is made in bleaching；Lignin liquor is carried out
Wine liquid is recycled in distillation；Lignin filtering will be precipitated, 27 kilograms of lignin is made in cleaning, drying；The wine liquid of recycling continues on for
Alcohol analysis, or it is used for distillate fuel ethyl alcohol；
By 65 kilograms of cellulose obtained above, ethyl alcohol is produced using acidic hydrolysis, 99.2% ethyl alcohol 9,000 is made
Gram, remaining 47 kilograms of fibers；
(7) it prepares liquid fertilizer: the activated carbon slag obtained after liquid pectin will be filtered out in step (4), and it is right in step (5)
Wine liquid distills out the mash slightly obtained after drinking and merges, and by pH value adjustment to 7, obtains 655 dry grams of liquid fertilizer.
2.3 kilograms of thick tannin, 38 kilograms of pectin, 47 kilograms of cellulose, 27 kilograms of lignin, ethyl alcohol is made in the present embodiment
81 kilograms and 655 kilograms of liquid fertilizer, recycle 107 kilograms of viable yeast mud.It is calculated, can get 2741 yuan of profits.
Embodiment 3:
(1) it prepares stalk silk: after the fresh sweet sorghum straw defoliation of acquisition, being sent into the sweet tea that pulverizer is ground into pipe tobacco shape
Broomcorn straw silk；
(2) extraction prepares tannin: by the methyl butyl as extractant of 1000 kilograms of sweet sorghum stalk silk and 700L
Ether is sent into fiberizer together, and guarantee sweet sorghum stalk silk and extractant uniformly, synchronous addition, be ground into the sweet tea height of 100 mesh
Fine strain of millet stalk slurry；
Sweet sorghum stalk slurry is put into fractionating column, stirs 15min, then stand 45min, extract liquor sufficiently divides with slurry
After layer, the extract liquor on fractionating tank top is pumped into distiller, extractant is recycled, obtains 2.3 kilograms of thick tannin；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, sweet sorghum stalk slurry of squeezing out
260 kilograms of 740 kilograms of syrup and sweet sorghum stalk slurry slag, then the sweet sorghum stalk slurry slag after squeezing is clear with 390 kilograms
After water impregnates, twice pressing, 405 kilograms of the syrup for sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slag 245 are carried out, and
The syrup squeezed out twice is mixed, 1145 kilograms of syrups are obtained, it is spare；
(4) it prepares pectin: by the sweet sorghum stalk slurry slag after twice pressing, being put into enamel reactor, and be added
The dilute sulfuric acid that 750L concentration is 5%；Then lead to and be steam heated to 80 DEG C, and keep the temperature 40min, make in sweet sorghum stalk slurry slag
Pectin dissolved well, then squeezed, separates pectin solution with sweet sorghum stalk slurry slag, obtain 770L pectin solution and
220 kilograms of sweet sorghum stalk slurry slag；1900g active carbon is added in the pectin solution squeezed out, decolourizes to pectin solution,
The liquid pectin obtained after filtering is added 539L, the ethyl alcohol that concentration is 95% in liquid pectin, pectin is precipitated；Then with centrifugation
Machine removes solution, extracts pectin；Pectin is cleaned, dry, pulverize, and 38 kilograms of pectin finished products are made；The solution pump that will be isolated
Enter distiller, recycles 75% ethyl alcohol 889L；Remaining acid solution 428L is used for subsequent pressurization acidolysis solution；
(5) it prepares xylose: the sweet sorghum stalk slurry slag (220kg) after pectin solution and residual will be squeezed in step (4)
Acid solution (428L) be uniformly mixed, and the sulfuric acid concentration of mixed material is adjusted to 3 ‰, is pumped into reactor tank, be passed through steam heating
To 115 DEG C, 90min is kept, pressurization acid hemolysis process is completed, makes hemicellulose fully degraded in acid solution, then leading to cold water makes instead
Tank is answered to be cooled to 100 DEG C hereinafter, syrup of squeezing out；By the syrup squeezed out by plus active carbon decoloring, ion exchange, nanofiltration,
9 kilograms of xylose is made in condensing crystallizing process；It is spare to collect the remaining residual sugar juice 110L of crystallization；
(6) prepare cellulose and lignin: the sweet sorghum stalk slurry slag (125kg) after squeezing syrup in step (5) is put
After the clear water immersion for entering 100L, dilute syrup (112L) is squeezed out；The investment of the sweet sorghum stalk slurry slag after dilute syrup will be squeezed out
In 6 times of material residue quality of 30% ethyl alcohol, and 556 grams of KOH are added as catalyst, after mixing, are sent into enamel reactor,
It is passed through steam heating, temperature is made to rise to 95 DEG C, 55min is kept, completes the pressurization alcoholysis process of slag charge, make the lignin of slag charge
Fully degraded；Then, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；
Cellulose slag charge is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, and 62 kilograms of cellulose is made in bleaching；To lignin liquor
It is distilled, recycles wine liquid；Lignin filtering will be precipitated, 26 kilograms of lignin is made in cleaning, drying；The wine liquid of recycling continues
It is analysed for alcohol, or is used for distillate fuel ethyl alcohol；
(7) prepare ethyl alcohol: the syrup that step (3), step (5) and step (6) are obtained mixes, and obtains syrup 1367L.Mixed
Ammonium hydroxide is added in syrup after conjunction, makes (NH in half congealed juice4)2SO4Content be 1g/L；Add the MgSO as nutritive salt4、
KH2PO4And CaCl2, respectively 14670g, 7335g and 7335g；Then white lime is added, the pH value of syrup is adjusted to 4.0；
The syrup 1370L modulated；88 kilograms of viable yeast mud of the recycling of embodiment 2, directly mix with the syrup of step (3), send
Enter fermentation bag and carry out anaerobic fermentation 36h, detects residual reducing sugar, less than 0.5%, alcoholic fermentation terminates content of reducing sugar；It will hair
Wine liquid after ferment is mature, is sent into distillation still, extracts 40% (v/v) thick wine by distillation, then 99.2% (v/ is extracted in rectifying, dehydration
V) 59 kilograms of alcohol fuel；90 kilograms of the viable yeast mud of retained sediments in fermentation bag, for next liquid glucose fermentation；
(8) it prepares liquid fertilizer: the activated carbon slag obtained after liquid pectin will be filtered out in step (4), step (5), with step
Suddenly the mash slightly obtained after drinking is distilled out in (7) to wine liquid to merge, and by pH value adjustment to 7, obtains 632 kilograms of liquid fertilizer.
2.3 kilograms of thick tannin, 38 kilograms of pectin, 63 kilograms of cellulose, 25 kilograms of lignin, ethyl alcohol is made in the present embodiment
59 kilograms, 9 kilograms of xylose and 632 kilograms of liquid fertilizer recycle 90 kilograms of viable yeast mud.It is calculated, processes 1 ton of fresh and sweet sorghum stalks
Stalk can get 2866 yuan of profits.
Embodiment 4:
(1) it prepares stalk silk: after the fresh sweet sorghum straw defoliation of acquisition, being sent into the sweet tea that pulverizer is ground into pipe tobacco shape
Broomcorn straw silk；
(2) extraction prepares tannin: taking 1000 kilograms of sweet sorghum stalk silk and the isopropyl ether one as extractant of 1000L
And be sent into fiberizer, and guarantee sweet sorghum stalk silk and extractant uniformly, it is synchronous add, be ground into the sugar grass straw of 100 mesh
Stalk slurry；
Sweet sorghum stalk slurry is put into fractionating column, stirs 150min, then stand 35min, extract liquor is abundant with slurry
After layering, the extract liquor on fractionating tank top is pumped into distiller, extractant is recycled, obtains 2.3 kilograms of thick tannin；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, sweet sorghum stalk slurry of squeezing out
262 kilograms of 738 kilograms of syrup and sweet sorghum stalk slurry slag, then the sweet sorghum stalk slurry slag after squeezing is clear with 315 kilograms
After water impregnates, twice pressing, 332 kilograms of the syrup for sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slag 245,000 are carried out
Gram, and the syrup squeezed out twice is mixed, 1070 kilograms of syrups are obtained, it is spare；
(4) it prepares pectin: by the sweet sorghum stalk slurry slag after twice pressing, being put into enamel reactor, and be added
The dilute syrup squeezed out in other batch steps (6) before 500L；Then lead to and be steam heated to 100 DEG C, and keep the temperature 20min, make
Pectin dissolved well in sweet sorghum stalk slurry slag, then squeezed, separate pectin solution with sweet sorghum stalk slurry slag,
Obtain the pectin solution of 540L and 210 kilograms of sweet sorghum stalk slurry slag；It is living that 2470g is added in the pectin solution squeezed out
Property charcoal, to pectin solution decolourize, the liquid pectin obtained after filtering, in liquid pectin be added 500L concentration be 95% ethyl alcohol, make
Pectin is precipitated；Then solution is removed with centrifuge, extracts pectin；Pectin is cleaned, dry, pulverize, be made 38 kilograms of pectin at
Product；The solution isolated is pumped into distiller, recycles 75% ethyl alcohol 633L；Remaining acid solution 341L, for subsequent pressurization acid
Solve solution；
(5) it prepares ethyl alcohol: the sweet sorghum stalk slurry slag after pectin solution will be squeezed in step (4) and remaining acid solution is mixed
It closes uniformly, and the sulfuric acid concentration of mixed material is adjusted to 5 ‰, be pumped into reactor tank, be passed through and be steam heated to 120 DEG C, keep
70min, completes pressurization acid hemolysis process, is substantially soluble in hemicellulose in acid solution, and then leading to cold water makes reactor tank be cooled to 100 DEG C
Hereinafter, syrup of squeezing out, obtains 170 kilograms of stalk slag；The syrup squeezed out is mixed with the syrup that step (3) is squeezed, upon mixing
Syrup in ammonium hydroxide is added, make (NH in half congealed juice4)2SO4Content be 1g/L；Add the MgSO as nutritive salt4、KH2PO4With
CaCl2, respectively 14110g, 7550g and 7550g；Then white lime is added, the pH value of syrup is adjusted to 5.0；It is modulated
Good syrup 1411L；
1/1100 syrup adjusted is taken, sugared concentration is adjusted to 2%；Add 460 grams of yeast of syrup 2/11000 after modulating,
Wherein, Angel Yeast and Candida utilis bacterium are respectively 322 grams and 138 grams.And saccharomycete oxygenation is given with sterile wind, carry out yeast expansion
Numerous, 120min expands numerous end.
Numerous rear yeast will be expanded to be sufficiently mixed with modulated syrup, fermentation bag is sent into, then closes fermentation bag and carry out anaerobism
Ferment 39h, detects residual reducing sugar content, less than 0.5%, alcoholic fermentation terminates content of reducing sugar；By the wine after fermenting-ripening
Liquid is sent into distillation still, extracts 40% (v/v) thick wine by distillation, then the alcohol fuel of 99.2% (v/v) is extracted in rectifying, dehydration
72 kilograms；97 kilograms of viable yeast mud for recycling retained sediments in fermentation bag, for next liquid glucose fermentation；
(6) prepare cellulose and lignin: 170 kilograms of sweet sorghum stalk slurry slag after squeezing syrup in step (5) is put
After the clear water immersion for entering 100L, dilute syrup is squeezed out；The sweet sorghum stalk slurry slag after dilute syrup will be squeezed out and put into material residue matter
In 30% ethyl alcohol of 5 times of amount, and 850 grams of KOH are added as catalyst, after mixing, are sent into enamel reactor, are passed through steaming
Vapour heating, makes temperature rise to 100 DEG C, keeps 60min, completes the pressurization alcoholysis process of slag charge, keep the lignin of slag charge abundant
Degradation；Then, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；Fiber
Plain slag charge is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, and 61 kilograms of cellulose is made in bleaching；Lignin liquor is carried out
Wine liquid is recycled in distillation；Lignin filtering will be precipitated, 23 kilograms of lignin is made in cleaning, drying；The wine liquid of recycling continues on for
Alcohol analysis, or it is used for distillate fuel ethyl alcohol；
(7) it prepares cellulosic ethanol: cellulose obtained in step (6) using cellulose degraded, then ferments, it is raw
11 kilograms of cellulosic ethanol are produced, 35 kilograms of residual fiber element；
(8) it prepares liquid fertilizer: the activated carbon slag obtained after liquid pectin will be filtered out in step (4), and it is right in step (5)
Wine liquid distills out the mash slightly obtained after drinking and merges, and by pH value adjustment to 7, obtains 479 kilograms of liquid fertilizer.
The present embodiment, be made 2.3 kilograms of thick tannin, 38 kilograms of pectin, 35 kilograms of cellulose, 11 kilograms of cellulosic ethanol,
23 kilograms of lignin, 72 kilograms of ethyl alcohol and 479 kilograms of liquid fertilizer recycle 97 kilograms of viable yeast mud.It is calculated, 1 ton of processing is fresh
Sweet sorghum stalk can get 2620.5 yuan of profits.
Claims (9)
1. a kind of method of sweet sorghum stalk comprehensive utilization, which is characterized in that comprise the steps of:
(1) it prepares stalk slurry: fresh and sweet broomcorn straw being removed into leaf, after crushing, is milled into the sweet sorghum stalk of 80 mesh or more
Slurry；
(2) extraction prepares tannin: sweet sorghum stalk slurry being put into fractionating column, extractant is added, the extractant of addition is ether
Class；The mass ratio of sweet sorghum stalk slurry and extractant is 1:0.7；After being sufficiently stirred, stratification；Upper layer of extraction liquid is pumped into
Distiller is distilled to recover extractant and tannin is made after extractant evaporation；
(3) it squeezes syrup: the slurry of fractionating column lower layer in step (2) being squeezed, the syrup for sweet sorghum stalk slurry of squeezing out,
After the sweet sorghum stalk slurry slag after squeezing is impregnated with clear water again, twice pressing is carried out, and the syrup squeezed out twice is mixed
It closes spare；
(4) it prepares pectin: the sweet sorghum stalk slurry slag after twice pressing being put into reactor tank, and dilute sulfuric acid is added, dilute sulphur
Acid concentration is 3~8 ‰, and the mass ratio of sweet sorghum stalk slurry slag and dilute sulfuric acid is 1:2.04~3.84；Then lead to steam heating
To 80~
100 DEG C, and 20~40min is kept the temperature, make the pectin dissolved well in sweet sorghum stalk slurry slag, then squeezed, makes fruit
Sol solution is separated with sweet sorghum stalk slurry slag；Active carbon is added in the pectin solution squeezed out, controls pectin solution dry
The mass ratio of matter and active carbon is 1:0.05~0.08, is decolourized to pectin solution, the liquid pectin obtained after filtering, in liquid pectin
The ethyl alcohol that concentration is 95% is added, the mass ratio for controlling liquid pectin and ethyl alcohol is 1:0.7~1.5, and pectin is precipitated；Then with from
Scheming removes solution, extracts pectin；Pectin is cleaned, dry, pulverize, and pectin finished product is made；The solution isolated is pumped into steaming
Device is evaporated, ethyl alcohol is recycled；Remaining acid solution is used for subsequent pressurization acidolysis solution；
(5) it prepares ethyl alcohol: the sweet sorghum stalk slurry slag after pectin solution will be squeezed in step (4) and mixed with remaining acid solution
It is even, and the sulfuric acid concentration of mixed material is adjusted to 3~8 ‰, it is pumped into reactor tank, is passed through and is steam heated to 115~125 DEG C, is protected
50~90min is held, pressurization acid hemolysis process is completed, makes hemicellulose fully degraded in acid solution, then leading to cold water drops reactor tank
Temperature is to 100 DEG C hereinafter, syrup of squeezing out；The syrup squeezed out is mixed with the syrup that step (3) is squeezed, in syrup upon mixing
Ammonium hydroxide is added, makes (NH in half congealed juice4)2S04Content be 1~1.5g/L；Nutritive salt is added, white lime is then added, by syrup
PH value adjust to 4~5；
1/1100~1/1000 of syrup quality after modulating is taken, the sugar aqueous solution that pol is 2% is diluted to, is put into yeast tank,
The saccharic alcohol Angel Yeast and candida utili of modulated syrup quality 2/11000~2/10000, saccharic wine are put into again
Smart Angel Yeast and candida utili are mixed in the ratio of 1~2.33:1, and with sterile wind to liquid glucose oxygenation dilute in yeast tank,
It carries out yeast and expands numerous, the numerous end of 120min expansion；
By modulated syrup and expand it is numerous after yeast juice be sent into fermentation bag, then close fermentation bag carry out anaerobic fermentation 30~
48h detects residual reducing sugar content, and less than 0.5%, alcoholic fermentation terminates content of reducing sugar；By the wine liquid after fermenting-ripening, send
Enter distillation still, extracts thick wine, then rectifying, dehydration by distillation, alcohol fuel is made；The viable yeast of retained sediments in fermentation bag
Mud, for next liquid glucose fermentation, after reusing 5~6 times, yeast activity decline is recycled yeast, is cleaned, dry, prepares yeast
Protein feed；
(6) cellulose and lignin are prepared: the sweet sorghum stalk slurry slag after squeezing syrup in step (5), after clear water impregnates,
Squeeze out dilute syrup；The sweet sorghum stalk slurry slag after dilute syrup will be squeezed out put into 4~6 times of material residue quality of 30% ethyl alcohol
In, and KOH is added as catalyst, and after mixing, it is sent into enamel reactor, it is closed, it is passed through steam heating, is made in temperature
95~105 DEG C are risen to, 55~65min is kept, completes the pressurization alcoholysis process of slag charge, make the lignin fully degraded of slag charge；So
Afterwards, lead to the cooling reactor tank of cold water, temperature is down to 50 DEG C hereinafter, squeezing out cellulose material residue and lignin liquor；Cellulose slag charge,
It is first cleaned with 30% ethyl alcohol, then is cleaned with clear water, cellulose is made in bleaching；Lignin liquor is distilled, wine liquid is recycled；
Lignin filtering will be precipitated, lignin is made in cleaning, drying；Recycling wine liquid continues on for alcohol analysis, or is used for distillate fuel second
Alcohol.
2. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (1)
In, when processing sweet sorghum stalk slurry, extractant is sent into fiberizer together with smashed sweet sorghum stalk, makes extractant
It is more abundant with the mixing of sweet sorghum stalk slurry.
3. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (3)
In, the mass ratio of sweet sorghum stalk slurry slag and clear water after squeezing is 1:1~1.5.
4. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that will be in step (4)
The activated carbon slag obtained after liquid pectin is filtered out, merges with the mash slightly obtained after drinking is distilled out to wine liquid in step (5), prepares
Liquid fertilizer.
5. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (5)
Middle nutritive salt is MgS04、KH2P04And CaCl2；In the syrup that every rising tune makes, MgS04、KH2P04And CaC12Additional amount difference
For 8~12g, 4~6g and 4~6g.
6. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (5)
In the syrup squeezed, or pass through decoloration, ion exchange, nanofiltration, condensing crystallizing process, the extraction higher wood of added value
Sugar；This is because the syrup main component squeezed out is xylose, in addition also contain arabinose, galactolipin, mannose.
7. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (6)
The middle KOH as catalyst, with squeeze out the sweet sorghum stalk stock quality ratio that 30% ethyl alcohol is added after dilute syrup be 1:900~
1100。
8. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (6)
In cellulose obtained, using cellulose degraded, then ferment, produce cellulosic ethanol.
9. a kind of method of sweet sorghum stalk comprehensive utilization according to claim 1, which is characterized in that above-mentioned steps (6)
In replace dilute sulfuric acid, sweet sorghum stalk slurry slag and dilute syrup in dilute syrup for squeezing out, or the step of being used for next batch (4)
Mass ratio be 1:4~6.
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| CN106222207A (en) * | 2016-08-10 | 2016-12-14 | 甘肃省科学院生物研究所 | A kind of sweet sorghum stalk fermentation fuel ethanol and the method for coproduction albumen feedstuff |
| CN106337063A (en) * | 2016-08-26 | 2017-01-18 | 内江师范学院 | Bitter gourd residue comprehensive utilization method |
| CN109336668A (en) * | 2018-08-23 | 2019-02-15 | 刘丰恺 | The extraction process of rice seedling raising ground substance plate cellulose |
| CN109776815A (en) * | 2019-03-27 | 2019-05-21 | 广州楹鼎生物科技有限公司 | A method of recycling lignin from solvent pulping bleaching waste liquor |
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