CN104109694A - Method for comprehensively utilizing sweet sorghum straws - Google Patents
Method for comprehensively utilizing sweet sorghum straws Download PDFInfo
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- CN104109694A CN104109694A CN201310660654.2A CN201310660654A CN104109694A CN 104109694 A CN104109694 A CN 104109694A CN 201310660654 A CN201310660654 A CN 201310660654A CN 104109694 A CN104109694 A CN 104109694A
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Abstract
The invention provides a method for comprehensively utilizing sweet sorghum straws. The method comprises the following steps: removing leaves from the sweet sorghum straws, crushing the leaf-removed sweet sorghum straws, grinding to form a slurry, and adding an extractant to obtain tannin; and preparing pectin, ethanol, cellulose and lignin in order to fully use the sweet sorghum straws. The method realizes the friendly processing environment, intensive processing and high processing efficiency of the sweet sorghum straws, fully utilizes useful substances in the sweet sorghum straws, increases the processing added values of the sweet sorghum straws, improves the resource utilization efficiency, realizes the zero emission of pollutants in the production process, is in favor of improving the sweet sorghum planting enthusiasm of peasant household, and powerfully promotes the raw material base construction of sweet sorghum.
Description
Technical field
The invention belongs to biological material and energy technology field, specifically, relate to a kind of method of sweet sorghum stalk comprehensive utilization.
Background technology
Sweet sorghum is one of farm crop that biological yield is the highest, in China, has long cultivation history, and all there is establishing in large scale in south and the north.The about cellulose 20～22% of fresh sweet sorghum stalk dry-matter, xylogen 10～12%, hemicellulose 16～19%, pectin 10～13%, crude protein 3～4%, total sugar content 35～41%, tannin 0.4～2.5%, crude fat, mineral substance etc. other 3～5%.
At present, sweet sorghum stalk utilization is mainly for the preparation of ethanol, through pilot scale economic balance, and high expensive, benefit is on the low side, all the time cannot Industry Promotion application.The comprehensive utilization of existing sweet sorghum stalk, at most just " ethanol-cardboard ", " ethanol-lees feeds ", " ethanol-wood sugar " coproduction, also not thorough to the utilization of sweet sorghum stalk useful matter, economic benefit fails to give full play to; As, the cardboard fiber making only reaches the level of making cardboard or carton, and the added value of lees feeds is lower, even extract wood sugar, economic benefit also awaits improving.Like this, both caused the wasting of resources, and produced again a large amount of discharges, cost of material can not get improving, and has a strong impact on the enthusiasm of Cotton Varieties by Small Farming Households sweet sorghum, and the scale in sugar grass raw material base cannot expand development, thereby has also restricted fuel ethanol industrial development.
Sweet sorghum is that plant few in number contains the higher C4 crop of tannin.Tannin also claims tannin extract, in industry widespread uses such as medicine, printing and dyeing, chemical industry, platform gold, wine brewing, stationery.It is to extract from blue or green persimmon and Turkey-galls that traditional tannin is produced, and the tannin that every production is 10,000 tons approximately need to be gone up persimmon or the Gallnut forest cultivated area of 100,000 mu.Because land resources is limited, traditional tannin extracting method cannot be met the need of market.Utilized in recent years pine needle and some wild plants to extract, but still cannot meet the need of market.If utilize sweet sorghum stalk to extract tannin, both can increase the added value of sweet sorghum stalk processing, also can supplement tannin market deficiency.In addition, ethanol, pectin, fiber, xylogen, feed are China's goods and materials in short supply." 12 " planning China promotes 5,000,000 tons of alcohol fuels, 3,000,000 tons of existing production capacity less thaies.Pectin, fiber and xylogen over nearly 10 years long-term dependence on import meet domestic market demand.China Sui Shi large agricultural country, grain-supply is but very nervous, is also that feed lacks country, and protein fodder especially lacks.With this, pull domestic demand, the above goods and materials in short supply of a large amount of development are produced, just the good opportunity of sweet sorghum stalk processing industry development.
Therefore, sweet sorghum stalk whole body is all precious.Fully extract sweet sorghum stalk useful component, not only its economic worth will become several times to increase, promote sweet sorghum stalk cost of material, improve the enthusiasm of Cotton Varieties by Small Farming Households sweet sorghum, drive sweet sorghum plant husbandry and relevant processing industry Sustainable development, and promoted fuel ethanol industrialization development, meanwhile, avoided the wasting of resources and a large amount of waste discharge.
Summary of the invention
For overcoming the deficiencies in the prior art part, the invention provides a kind of method of sweet sorghum stalk comprehensive utilization, combination producing ethanol, tannin, pectin, fiber, xylogen, thereby reduce the comprehensive utilization cost of sweet sorghum stalk, increase sweet sorghum stalk processing added value, improve the level of resources utilization, realize production process zero release of pollutant.
The technical solution adopted for the present invention to solve the technical problems is that the method for sweet sorghum stalk comprehensive utilization, comprises following steps:
(1) prepare stalk slurry: fresh and sweet broomcorn straw is removed to leaf, after pulverizing, grind into sweet sorghum stalk slurries more than 80 orders;
(2) tannin is prepared in extraction: sweet sorghum stalk slurry is dropped in separation column, add extraction agent, and after fully stirring, stratification; Upper layer of extraction liquid is pumped into distiller, and Distillation recovery extraction agent, after extraction agent evaporation, makes tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, the squeeze out syrup of sweet sorghum stalk slurry, after again the sweet sorghum stalk slurry slag after squeezing being soaked with clear water, carry out twice pressing, and by the syrup mixing for standby use squeezing out for twice;
(4) prepare pectin: the sweet sorghum stalk slurry slag after twice pressing is put into retort, and add dilute sulphuric acid; Then lead to and be steam heated to 80～100 ℃, and be incubated 20～40min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag; In the pectin solution squeezing out, add gac, to pectin solution decolouring, the liquid pectin obtaining after filtering adds ethanol in liquid pectin, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes pectin finished product; Isolated solution is pumped into distiller, reclaim ethanol; Residual acid solution, for follow-up pressurization acidolysis solution;
(5) prepare ethanol: the sweet sorghum stalk slurry slag squeezing in step (4) after pectin solution is mixed with residual acid solution, and the sulfuric acid concentration of mixture is adjusted to 3～8 ‰, pump into retort, pass into and be steam heated to 115～125 ℃, keep 50～90min, complete pressurization acidolysis process, hemicellulose is fully degraded in acid solution, then logical cold water is cooled to below 100 ℃ retort, the syrup of squeezing out; The syrup that the syrup of squeezing out is squeezed with step (3) is mixed, and in mixed syrup, adds ammoniacal liquor, makes (NH in half congealed juice
4)
2sO
4content be 1～1.5g/L; Add again nutritive salt, then add white lime, the pH value of syrup is adjusted to 4～5;
Get 1/1100～1/900 of the rear syrup quality of modulation, be diluted to pol and be 2% sugar aqueous solution, drop in yeast tank, drop into again saccharic alcohol Angel Yeast and the Candida utilis of the syrup quality 2/11000～2/9000 after modulation, saccharic alcohol Angel Yeast and Candida utilis mix in the ratio of 5～8:2～5, and with sterile wind to rare liquid glucose oxygenation in yeast tank, carry out yeast and expand numerously, 100～150min expands numerous end;
Yeast juice after syrup after modulation and expansion is numerous is sent into fermentation bag, then seals fermentation bag and carries out anaerobically fermenting 30～48h, detects remaining reducing sugar content, and reducing sugar content is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through distillation extraction thick wine, then rectifying, dehydration, make alcohol fuel; The viable yeast mud of residual precipitation in fermentation bag, for next liquid glucose fermentation, reuses after 5～6 times, and yeast activity declines, and reclaims yeast, cleans, dry, prepares Yeast protein feed;
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze the sweet sorghum stalk slurry slag after syrup, after clear water soaks, squeeze out rare syrup; The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 4～6 times of material slag amounts, and add KOH as catalyzer, after mixing, send in enamel reactor, airtight, pass into steam heating, make temperature rise to 95～105 ℃, keep 55～65min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes Mierocrystalline cellulose; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make xylogen; Recovery wine liquid continues on for alcohol and analyses, or for distillate fuel ethanol.
In above-mentioned steps (1), during processing sweet sorghum stalk slurry, extraction agent is sent in paste roller mill with together with sweet sorghum stalk after pulverizing, made extraction agent more abundant with mixing of sweet sorghum stalk slurry.
The extraction agent adding in above-mentioned steps (2) is ethers; The mass ratio of sweet sorghum stalk slurry and extraction agent is 1:0.7～1.1.
In above-mentioned steps (3), the sweet sorghum stalk slurry slag after squeezing and the mass ratio of clear water are 1:1～1.5.
Dilute sulphuric acid concentration in above-mentioned steps (4) is 3～8 ‰, and the mass ratio of sweet sorghum stalk slurry slag and dilute sulphuric acid is 1:2.04～3.84; The mass ratio of pectin solution dry-matter and gac is 1:0.05～0.08; The concentration of ethanol is 95%, and the mass ratio of liquid pectin and ethanol is 1:0.7～1.5.
To in step (4), filter out the activated carbon slag obtaining after liquid pectin, and in step (5), wine liquid is distilled out to the mash slightly obtaining after drinking and merge, prepare liquid fertilizer.
In above-mentioned steps (5), nutritive salt is MgSO
4, KH
2pO
4and CaCl
2; In the syrup that every rising tune makes, MgSO
4, KH
2pO
4and CaCl
2add-on be respectively 8～12g, 4～6g and 4～6g.
The syrup of squeezing in above-mentioned steps (5), or through decolouring, ion-exchange, nanometer ultrafiltration, condensing crystal operation, extract the higher wood sugar of added value; This is because the syrup main component of squeezing out is wood sugar, in addition also containing pectinose, semi-lactosi, seminose.
In above-mentioned steps (6) as the KOH of catalyzer, with squeeze out rare syrup after add the sweet sorghum stalk stock quality of 3O% ethanol than being 1:900～1100.
The Mierocrystalline cellulose making in above-mentioned steps (6), adopts cellulose degraded, then ferments, production of cellulosic ethanol.
Rare syrup of squeezing out in above-mentioned steps (6), or replace dilute sulphuric acid for the step (4) of next batch, the mass ratio of sweet sorghum stalk slurry slag and rare syrup is 1:4～6.
The method of sweet sorghum stalk comprehensive utilization of the present invention, makes tannin, pectin, ethanol, fiber and xylogen in stalk obtain utilizing fully, and has reclaimed yeast, with existing sweet sorghum stalk processing technology, compares, and has following advantage:
Compare with existing " solid fermentation method ", " fermentation method of squeezing the juice ", the present invention not only utilizes glucose, fructose, the sucrose of sweet sorghum stalk, has also utilized wood sugar, the seminose fermenting alcohol of half fiber degradation, and alcohol yied increases substantially.
Compare with existing " beating method ", the present invention is on the basis of to succeed and develop " beating method " superiority, integrated " abstraction technique ", " acidolysis technology " and " alcoholysis technology ", further excavate the utility value of sweet sorghum stalk resource, fully extracted the useful component of sweet sorghum stalk, sweet sorghum stalk is developed from refining ethanol single product, change exploitation multiple product into, increased substantially the economic benefit of the stalk deep processings such as sweet sorghum.
Compare with existing " ethanol-cardboard ", " ethanol-lees feeds ", " ethanol-wood sugar " comprehensive use, the present invention is on the basis of integrated multinomial technology, from sweet sorghum stalk, extract tannin, ethanol, pectin, fiber, xylogen, and reclaimed the multiple products such as yeast.Meanwhile, the present invention has taken into full account the unification of sweet sorghum stalk processing with ecological environmental protection, has used in process of production medicament and the solvent that can be converted into fertilizer, has accomplished that all waste liquids, waste residue are all converted into fertilizer.
Therefore, the present invention has realized sweet sorghum stalk processing environment close friend and intensive efficient target, takes full advantage of the useful matter in sweet sorghum stalk, has increased sweet sorghum stalk processing added value, improve the level of resources utilization, realized production process zero release of pollutant.Be conducive to improve the enthusiasm of Cotton Varieties by Small Farming Households sweet sorghum, and will effectively promote the raw material site construction of sweet sorghum.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
(1) prepare stalk slurry: by after the fresh sweet sorghum straw defoliation gathering, send into the sweet sorghum stalk silk that pulverizer is ground into pipe tobacco shape, get 1000 kilograms of stalk silks, measuring its moisture content is 75%, and dry matter content is 25%; In dry-matter, total Soluble Sugar content is 48%, approximately 120 kilograms; Other slag charge accounts for 52%, approximately 130 kilograms; Again sweet sorghum stalk silk is sent into paste roller mill and pumped into 1100 kilograms of propyl ether simultaneously, grind to form 100 object sweet sorghum stalk mixed slurries;
(2) tannin is prepared in extraction: sweet sorghum stalk mixed slurry is dropped in separation column, stir 20min, more standing 60min, after the abundant layering of extraction liquid and slurry, by the extraction liquid suction distiller on fractionating tank top, reclaim extraction agent, obtain 2.3 kilograms of thick tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, 260 kilograms of 740 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, after again the sweet sorghum stalk slurry slag after squeezing being soaked with 260 kilograms of clear water, carry out twice pressing, 245 kilograms of 275 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, and the syrup squeezing out for twice is mixed, obtain altogether 1015 kilograms of syrups, standby;
(4) prepare pectin: by the sweet sorghum stalk slurry slag after twice pressing, put into enamel reactor, and to add 500L concentration be 0.8% dilute sulphuric acid; Then lead to and be steam heated to 100 ℃, and be incubated 20min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag, obtain the pectin solution of 450L and the sweet sorghum stalk slurry slag of 210 kilograms; In the pectin solution squeezing out, add 3040g gac, to pectin solution decolouring, the liquid pectin obtaining after filtering adds the ethanol that 675L, concentration are 95% in liquid pectin, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes 38 kilograms of pectin finished products; Isolated solution is pumped into distiller, reclaim 75% ethanol 850L; Residual acid solution 270L, for follow-up pressurization acidolysis solution;
(5) prepare ethanol: by squeezing 210 kilograms of sweet sorghum stalk slurry slags after pectin solution in step (4), mix with residual acid solution (270L), and the sulfuric acid concentration of mixture is adjusted to 8 ‰, pump into retort, pass into and be steam heated to 125 ℃, keep 50min, complete pressurization acidolysis process, make hemicellulose fully be dissolved in acid solution, then logical cold water is cooled to below 100 ℃ retort, the syrup of squeezing out 320L, 176 kilograms of slag charges; The syrup that the syrup of squeezing out is squeezed with step (3) is mixed, and in mixed syrup, adds ammoniacal liquor, makes (NH in half congealed juice
4)
2sO
4content be 1.5g/L; Add again the MgSO as nutritive salt
4, KH
2pO
4and CaCl
2, be respectively 11850g, 5900g and 5900g; Then add white lime, the pH value of syrup is adjusted to 5; The syrup 1335L that obtains modulating;
Get the syrup 14.83L after 1/900 modulation, it is 2% sugar aqueous solution that thin up becomes pol, drop in yeast tank, drop into again 240 grams, the yeast of the syrup quality 2/11000 after modulation, wherein saccharic alcohol Angel Yeast and Candida utilis are respectively 192 grams and 48 grams, and with sterile wind to rare liquid glucose oxygenation in tank, carry out yeast and expand numerously, about 150min expands numerous end;
Yeast juice after syrup after modulation and expansion is numerous is sent into fermentation bag, then seals fermentation bag and carries out anaerobically fermenting 48h, detects remaining reducing sugar content, is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through the thick wine of distillation extraction 40% (v/v), then 72 kilograms of the alcohol fuels of 99.2% (v/v) are extracted in rectifying, dehydration; Reclaim 97 kilograms, the viable yeast mud of residual precipitation in fermentation bag, for the fermentation of next batch liquid glucose (after recycling 6 times, yeast activity declines, and reclaims yeast, cleans, dry, for making dry yeast protein fodder);
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze 176 kilograms of sweet sorghum stalk slurry slags after syrup, after the clear water of putting into 100L soaks, squeeze out rare syrup; The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 5 times of material slag amounts, and add 978 grams of KOH as catalyzer, after mixing, send in enamel reactor, pass into steam heating, make temperature rise to 105 ℃, keep 55min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes the Mierocrystalline cellulose of 63 kilograms; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make 25 kilograms, xylogen; The wine liquid reclaiming is analysed for the alcohol of next production batch, or for distillate fuel ethanol;
(7) prepare liquid fertilizer: the activated carbon slag obtaining after liquid pectin will be filtered out in step (4), and in step (5), wine liquid is distilled out to the mash slightly obtaining after drinking and merge, and pH value is adjusted to 7, obtain 432 kilograms of liquid fertilizers.
The present embodiment, makes 432 kilograms of 2.3 kilograms of thick tannin, 38 kilograms of pectin, 63 kilograms of Mierocrystalline celluloses, 25 kilograms, xylogen, 72 kilograms of ethanol and liquid fertilizers, reclaims 97 kilograms, viable yeast mud.Through adjusting, process 1 ton of fresh and sweet broomcorn straw, can obtain 2642 yuan of profits.
Embodiment 2:
(1) prepare stalk slurry: after the fresh sweet sorghum straw defoliation of collection, send into the sweet sorghum stalk silk that pulverizer is ground into pipe tobacco shape; Getting the sweet sorghum stalk silk of 1000 kilograms sends into paste mill grinding machine and grinds to form 100 object sweet sorghum stalk slurries;
(2) tannin is prepared in extraction: sweet sorghum stalk slurry is dropped in separation column, add the allyl ethyl ether of 900L as extraction agent, stir 10min, standing 30min again, after the abundant layering of extraction liquid and slurry, by the extraction liquid suction distiller on fractionating tank top, reclaim extraction agent, obtain 2.1 kilograms of thick tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, 265 kilograms of 735 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, after again the sweet sorghum stalk slurry slag after squeezing being soaked with 300 kilograms of clear water, carry out twice pressing, 260 kilograms of 320 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, and the syrup squeezing out for twice is mixed, obtain altogether 1055 kilograms of syrups, standby;
(4) prepare pectin: by the sweet sorghum stalk slurry slag after twice pressing, put into enamel reactor, and to add 1000L concentration be 5% dilute sulphuric acid; Then lead to and be steam heated to 90 ℃, and be incubated 30min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag, obtain the pectin solution of 810L and the sweet sorghum stalk slurry slag of 215 kilograms; In the pectin solution squeezing out, add 2535g gac, to pectin solution decolouring, the liquid pectin obtaining after filtering, in liquid pectin, adding 891L concentration is 95% ethanol, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes 39 kilograms of pectin finished products; Isolated solution is pumped into distiller, reclaim 75% ethanol 1131L; Residual acid solution 570L, for follow-up pressurization acidolysis solution;
(5) prepare ethanol: by squeezing 215 kilograms of sweet sorghum stalk slurry slags after pectin solution in step (4), mix with residual acid solution 570L, and the sulfuric acid concentration of mixture is adjusted to 5 ‰, pump into retort, pass into and be steam heated to 120 ℃, keep 70min, complete pressurization acidolysis process, make hemicellulose fully be dissolved in acid solution, then logical cold water is cooled to below 100 ℃ retort, the syrup of squeezing out 530L; The syrup that the syrup of squeezing out is squeezed with step (3) is mixed, and in mixed syrup, adds ammoniacal liquor, makes (NH in half congealed juice
4)
2sO
4content be 1.25g/L; Add again the MgSO as nutritive salt
4, KH
2pO
4and CaCl
2, be respectively 15850g, 7900g and 7900g; Then add white lime, the pH value of syrup is adjusted to 4.5; The syrup 1585L that obtains modulating;
Get 1/1000 syrup of adjusting, sugared concentration is adjusted to 2%; 288 grams, the yeast that adds syrup 2/10000 after modulation, wherein, Angel Yeast and Candida utilis bacterium are respectively 144 grams and 144 grams.And with sterile wind to yeast oxygenation, carry out yeast and expand numerously, 120min expands numerous end.
Yeast after expansion is numerous and the syrup after modulation are sent into fermentation bag after fully mixing, and then seal fermentation bag and carry out anaerobically fermenting 39h, detect remaining reducing sugar content, and reducing sugar content is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through the thick wine of distillation extraction 40% (v/v), then 72 kilograms of the alcohol fuels of 99.2% (v/v) are extracted in rectifying, dehydration; 107 kilograms, the viable yeast mud of the interior residual precipitation of recovery fermentation bag, ferments for next batch liquid glucose;
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze 180 kilograms of sweet sorghum stalk slurry slags after syrup, after the clear water of putting into 100L soaks, squeeze out rare syrup; The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 5 times of material slag amounts, and add 900 grams of KOH as catalyzer, after mixing, send in enamel reactor, pass into steam heating, make temperature rise to 100 ℃, keep 60min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes the Mierocrystalline cellulose of 65 kilograms; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make 27 kilograms, xylogen; The wine liquid reclaiming continues on for alcohol and analyses, or for distillate fuel ethanol;
By the above-mentioned Mierocrystalline cellulose of 65 kilograms making, adopt acidic hydrolysis to produce ethanol, make 9 kilograms of 99.2% ethanol, residue 47 kg of fibers;
(7) prepare liquid fertilizer: the activated carbon slag obtaining after liquid pectin will be filtered out in step (4), and in step (5), wine liquid is distilled out to the mash slightly obtaining after drinking and merge, and pH value is adjusted to 7, obtain dry gram of liquid fertilizer 655.
The present embodiment, makes 655 kilograms of 2.3 kilograms of thick tannin, 38 kilograms of pectin, 47 kilograms of Mierocrystalline celluloses, 27 kilograms, xylogen, 81 kilograms of ethanol and liquid fertilizers, reclaims 107 kilograms, viable yeast mud.Through adjusting, can obtain 2741 yuan of profits.
Embodiment 3:
(1) prepare stalk silk: after the fresh sweet sorghum straw defoliation of collection, send into the sweet sorghum stalk silk that pulverizer is ground into pipe tobacco shape;
(2) tannin is prepared in extraction: the methyl butyl ether as extraction agent of the sweet sorghum stalk silk of 1000 kilograms and 700L is sent in paste roller mill in the lump, and guarantee sweet sorghum stalk silk and extraction agent evenly, synchronize interpolation, grind to form 100 object sweet sorghum stalk slurries;
Sweet sorghum stalk slurry is dropped in separation column, stir 15min, more standing 45min, after the abundant layering of extraction liquid and slurry, by the extraction liquid suction distiller on fractionating tank top, reclaim extraction agent, obtain 2.3 kilograms of thick tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, 260 kilograms of 740 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, after again the sweet sorghum stalk slurry slag after squeezing being soaked with 390 kilograms of clear water, carry out twice pressing, squeeze out 405 kilograms of syrups and the sweet sorghum stalk slurry slag 245 of sweet sorghum stalk slurry, and the syrup squeezing out for twice is mixed, obtain altogether 1145 kilograms of syrups, standby;
(4) prepare pectin: by the sweet sorghum stalk slurry slag after twice pressing, put into enamel reactor, and to add 750L concentration be 5% dilute sulphuric acid; Then lead to and be steam heated to 80 ℃, and be incubated 40min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag, obtain the pectin solution of 770L and the sweet sorghum stalk slurry slag of 220 kilograms; In the pectin solution squeezing out, add 1900g gac, to pectin solution decolouring, the liquid pectin obtaining after filtering adds the ethanol that 539L, concentration are 95% in liquid pectin, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes 38 kilograms of pectin finished products; Isolated solution is pumped into distiller, reclaim 75% ethanol 889L; Residual acid solution 428L, for follow-up pressurization acidolysis solution;
(5) prepare wood sugar: the sweet sorghum stalk slurry slag (220kg) squeezing in step (4) after pectin solution is mixed with residual acid solution (428L), and the sulfuric acid concentration of mixture is adjusted to 3 ‰, pump into retort, pass into and be steam heated to 115 ℃, keep 90min, complete pressurization acidolysis process, hemicellulose is fully degraded in acid solution, then logical cold water is cooled to below 100 ℃ retort, the syrup of squeezing out; The syrup of squeezing out, through adding activated carbon decolorizing, ion-exchange, nanometer ultrafiltration, condensing crystal operation, is made to the wood sugar of 9 kilograms; Collect crystallization residue residual sugar juice 110L standby;
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze the sweet sorghum stalk slurry slag (125kg) after syrup, put into after the clear water immersion of 100L, squeeze out rare syrup (112L); The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 6 times of material slag amounts, and add 556 grams of KOH as catalyzer, after mixing, send in enamel reactor, pass into steam heating, make temperature rise to 95 ℃, keep 55min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes the Mierocrystalline cellulose of 62 kilograms; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make 26 kilograms, xylogen; The wine liquid reclaiming continues on for alcohol and analyses, or for distillate fuel ethanol;
(7) prepare ethanol: the syrup that step (3), step (5) and step (6) are obtained is mixed, and obtains syrup 1367L.In mixed syrup, add ammoniacal liquor, make (NH in half congealed juice
4)
2sO
4content be 1g/L; Add again the MgSO as nutritive salt
4, KH
2pO
4and CaCl
2, be respectively 14670g, 7335g and 7335g; Then add white lime, the pH value of syrup is adjusted to 4.0; The syrup 1370L that obtains modulating; 88 kilograms, the viable yeast mud that embodiment 2 reclaims, directly mixes with the syrup of step (3), sends into fermentation bag and carries out anaerobically fermenting 36h, detects remaining reducing sugar, and reducing sugar content is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through the thick wine of distillation extraction 40% (v/v), then 59 kilograms of the alcohol fuels of 99.2% (v/v) are extracted in rectifying, dehydration; 90 kilograms, the viable yeast mud of the interior residual precipitation of fermentation bag, for next liquid glucose fermentation;
(8) prepare liquid fertilizer: will in step (4), step (5), filter out the activated carbon slag obtaining after liquid pectin, with in step (7), wine liquid is distilled out to the mash slightly obtaining after drinking and merges, and pH value is adjusted to 7, obtain 632 kilograms of liquid fertilizers.
The present embodiment, makes 632 kilograms of 2.3 kilograms of thick tannin, 38 kilograms of pectin, 63 kilograms of Mierocrystalline celluloses, 25 kilograms, xylogen, 59 kilograms of ethanol, 9 kilograms of wood sugars and liquid fertilizers, reclaims 90 kilograms, viable yeast mud.Through adjusting, process 1 ton of fresh and sweet broomcorn straw, can obtain 2866 yuan of profits.
Embodiment 4:
(1) prepare stalk silk: after the fresh sweet sorghum straw defoliation of collection, send into the sweet sorghum stalk silk that pulverizer is ground into pipe tobacco shape;
(2) tannin is prepared in extraction: get the sweet sorghum stalk silk of 1000 kilograms and the isopropyl ether as extraction agent of 1000L and send in paste roller mill in the lump, and guarantee sweet sorghum stalk silk and extraction agent evenly, synchronize interpolation, grind to form 100 object sweet sorghum stalk slurries;
Sweet sorghum stalk slurry is dropped in separation column, stir 150min, more standing 35min, after the abundant layering of extraction liquid and slurry, by the extraction liquid suction distiller on fractionating tank top, reclaim extraction agent, obtain 2.3 kilograms of thick tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, 262 kilograms of 738 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, after again the sweet sorghum stalk slurry slag after squeezing being soaked with 315 kilograms of clear water, carry out twice pressing, 245 kilograms of 332 kilograms of the syrups of sweet sorghum stalk slurry of squeezing out and sweet sorghum stalk slurry slags, and the syrup squeezing out for twice is mixed, obtain altogether 1070 kilograms of syrups, standby;
(4) prepare pectin: by the sweet sorghum stalk slurry slag after twice pressing, put into enamel reactor, and add rare syrup of squeezing out in other batch of step (6) before 500L; Then lead to and be steam heated to 100 ℃, and be incubated 20min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag, obtain the pectin solution of 540L and the sweet sorghum stalk slurry slag of 210 kilograms; In the pectin solution squeezing out, add 2470g gac, to pectin solution decolouring, the liquid pectin obtaining after filtering, in liquid pectin, adding 500L concentration is 95% ethanol, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes 38 kilograms of pectin finished products; Isolated solution is pumped into distiller, reclaim 75% ethanol 633L; Residual acid solution 341L, for follow-up pressurization acidolysis solution;
(5) prepare ethanol: the sweet sorghum stalk slurry slag squeezing in step (4) after pectin solution is mixed with residual acid solution, and the sulfuric acid concentration of mixture is adjusted to 5 ‰, pump into retort, pass into and be steam heated to 120 ℃, keep 70min, complete pressurization acidolysis process, make hemicellulose fully be dissolved in acid solution, then logical cold water is cooled to below 100 ℃ retort, and the syrup of squeezing out, obtains 170 kilograms of stalk slags; The syrup that the syrup of squeezing out is squeezed with step (3) is mixed, and in mixed syrup, adds ammoniacal liquor, makes (NH in half congealed juice
4)
2sO
4content be 1g/L; Add again the MgSO as nutritive salt
4, KH
2pO
4and CaCl
2, be respectively 14110g, 7550g and 7550g; Then add white lime, the pH value of syrup is adjusted to 5.0; The syrup 1411L that obtains modulating;
Get 1/1100 syrup of adjusting, sugared concentration is adjusted to 2%; 460 grams, the yeast that adds syrup 2/11000 after modulation, wherein, Angel Yeast and Candida utilis bacterium are respectively 322 grams and 138 grams.And with sterile wind to yeast oxygenation, carry out yeast and expand numerously, 120min expands numerous end.
By expanding numerous rear yeast, fully mix with the syrup after modulation, send into fermentation bag, then seal fermentation bag and carry out anaerobically fermenting 39h, detect remaining reducing sugar content, reducing sugar content is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through the thick wine of distillation extraction 40% (v/v), then 72 kilograms of the alcohol fuels of 99.2% (v/v) are extracted in rectifying, dehydration; 97 kilograms, the viable yeast mud of the interior residual precipitation of recovery fermentation bag, for next liquid glucose fermentation;
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze 170 kilograms of sweet sorghum stalk slurry slags after syrup, after the clear water of putting into 100L soaks, squeeze out rare syrup; The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 5 times of material slag amounts, and add 850 grams of KOH as catalyzer, after mixing, send in enamel reactor, pass into steam heating, make temperature rise to 100 ℃, keep 60min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes the Mierocrystalline cellulose of 61 kilograms; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make 23 kilograms, xylogen; The wine liquid reclaiming continues on for alcohol and analyses, or for distillate fuel ethanol;
(7) prepare cellulosic ethanol: by the Mierocrystalline cellulose making in step (6), adopt cellulose degraded, then ferment, 11 kilograms of production of cellulosic ethanol, 35 kilograms of residual fiber elements;
(8) prepare liquid fertilizer: the activated carbon slag obtaining after liquid pectin will be filtered out in step (4), and in step (5), wine liquid is distilled out to the mash slightly obtaining after drinking and merge, and pH value is adjusted to 7, obtain 479 kilograms of liquid fertilizers.
The present embodiment, makes 479 kilograms of 2.3 kilograms of thick tannin, 38 kilograms of pectin, 35 kilograms of Mierocrystalline celluloses, 11 kilograms of cellulosic ethanols, 23 kilograms, xylogen, 72 kilograms of ethanol and liquid fertilizers, reclaims 97 kilograms, viable yeast mud.Through adjusting, process 1 ton of fresh and sweet broomcorn straw, can obtain 2620.5 yuan of profits.
Claims (11)
1. a method for sweet sorghum straw comprehensive utilization, is characterized in that, comprises following steps:
(1) prepare stalk slurry: fresh and sweet broomcorn straw is removed to leaf, after pulverizing, grind into sweet sorghum stalk slurries more than 80 orders;
(2) tannin is prepared in extraction: sweet sorghum stalk slurry is dropped in separation column, add extraction agent, and after fully stirring, stratification; Upper layer of extraction liquid is pumped into distiller, and Distillation recovery extraction agent, after extraction agent evaporation, makes tannin;
(3) squeeze syrup: the slurry to separation column lower floor in step (2) squeezes, the squeeze out syrup of sweet sorghum stalk slurry, after again the sweet sorghum stalk slurry slag after squeezing being soaked with clear water, carry out twice pressing, and by the syrup mixing for standby use squeezing out for twice;
(4) prepare pectin: the sweet sorghum stalk slurry slag after twice pressing is put into retort, and add dilute sulphuric acid; Then lead to and be steam heated to 80～100 ℃, and be incubated 20～40min, the pectin in sweet sorghum stalk slurry slag is fully dissolved, then squeeze, make pectin solution separated with sweet sorghum stalk slurry slag; In the pectin solution squeezing out, add gac, to pectin solution decolouring, the liquid pectin obtaining after filtering adds ethanol in liquid pectin, and pectin is separated out; Then with whizzer, remove solution, extract pectin; Pectin, through cleaning, dry, pulverize, and makes pectin finished product; Isolated solution is pumped into distiller, reclaim ethanol; Residual acid solution, for follow-up pressurization acidolysis solution;
(5) prepare ethanol: the sweet sorghum stalk slurry slag squeezing in step (4) after pectin solution is mixed with residual acid solution, and the sulfuric acid concentration of mixture is adjusted to 3～8 ‰, pump into retort, pass into and be steam heated to 115～125 ℃, keep 50～90min, complete pressurization acidolysis process, hemicellulose is fully degraded in acid solution, then logical cold water is cooled to below 100 ℃ retort, the syrup of squeezing out; The syrup that the syrup of squeezing out is squeezed with step (3) is mixed, and in mixed syrup, adds ammoniacal liquor, and the content that makes (NH4) 2S04 in half congealed juice is 1～1.5g/L; Add again nutritive salt, then add white lime, the pH value of syrup is adjusted to 4～5;
Get 1/1100～1/900 of the rear syrup quality of modulation, be diluted to pol and be 2% sugar aqueous solution, drop in yeast tank, drop into again saccharic alcohol Angel Yeast and the Candida utilis of the syrup quality 2/11000～2/9000 after modulation, saccharic alcohol Angel Yeast and Candida utilis mix in the ratio of 5～8:2～5, and with sterile wind to rare liquid glucose oxygenation in yeast tank, carry out yeast and expand numerously, 100～150min expands numerous end;
Yeast juice after syrup after modulation and expansion is numerous is sent into fermentation bag, then seals fermentation bag and carries out anaerobically fermenting 30～48h, detects remaining reducing sugar content, and reducing sugar content is less than 0.5%, and zymamsis finishes; By the wine liquid after fermenting-ripening, send into still kettle, through distillation extraction thick wine, then rectifying, dehydration, make alcohol fuel; The viable yeast mud of residual precipitation in fermentation bag, for next liquid glucose fermentation, reuses after 5～6 times, and yeast activity declines, and reclaims yeast, cleans, dry, prepares Yeast protein feed;
(6) prepare Mierocrystalline cellulose and xylogen: in step (5), squeeze the sweet sorghum stalk slurry slag after syrup, after clear water soaks, squeeze out rare syrup; The sweet sorghum stalk slurry slag squeezing out after rare syrup is dropped in 30% ethanol of 4～6 times of material slag amounts, and add KOH as catalyzer, after mixing, send in enamel reactor, airtight, pass into steam heating, make temperature rise to 95～105 ℃, keep 55～65min, complete the pressurization alcoholysis process of slag charge, the xylogen of slag charge is fully degraded; Then, the logical cooling retort of cold water, temperature is down to below 50 ℃, squeezes out Mierocrystalline cellulose material slag and lignin liquor; Mierocrystalline cellulose slag charge, first cleans with 30% ethanol, then cleans with clear water, and bleaching, makes Mierocrystalline cellulose; Lignin liquor is distilled, reclaim wine liquid; To separate out xylogen and filter, cleaning, drying, make xylogen; Recovery wine liquid continues on for alcohol and analyses, or for distillate fuel ethanol.
2. the method that a kind of sweet sorghum straw according to claim 1 fully utilizes, it is characterized in that, in above-mentioned steps (1), during processing sweet sorghum stalk slurry, extraction agent is sent in paste roller mill with together with sweet sorghum stalk after pulverizing, made extraction agent more abundant with mixing of sweet sorghum stalk slurry.
3. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, the extraction agent adding in above-mentioned steps (2) is ethers; The mass ratio of sweet sorghum stalk slurry and extraction agent is 1:0.7～1.1.
4. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, in above-mentioned steps (3), the sweet sorghum stalk slurry slag after squeezing and the mass ratio of clear water are 1:1～1.5.
5. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, the dilute sulphuric acid concentration in above-mentioned steps (4) is 3～8 ‰, and the mass ratio of sweet sorghum stalk slurry slag and dilute sulphuric acid is 1:2.04～3.84; The mass ratio of pectin solution dry-matter and gac is 1:0.05～0.08; The concentration of ethanol is 95%, and the mass ratio of liquid pectin and ethanol is 1:0.7～1.5.
6. the method that a kind of sweet sorghum straw according to claim 1 fully utilizes, it is characterized in that, to in step (4), filter out the activated carbon slag obtaining after liquid pectin, and in step (5), wine liquid is distilled out to the mash slightly obtaining after drinking and merge, prepare liquid fertilizer.
7. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, in above-mentioned steps (5), nutritive salt is MgS04, KH2P04 and CaCl2; In the syrup that every rising tune makes, the add-on of MgS04, KH2P04 and CaC12 is respectively 8～12g, 4～6g and 4～6g.
8. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, the syrup of squeezing in above-mentioned steps (5), or through decolouring, ion-exchange, nanometer ultrafiltration, condensing crystal operation, extract the higher wood sugar of added value; This is because the syrup main component of squeezing out is wood sugar, in addition also containing pectinose, semi-lactosi, seminose.
9. the method that a kind of sweet sorghum straw according to claim 1 fully utilizes, it is characterized in that, in above-mentioned steps (6) as the KOH of catalyzer, with squeeze out rare syrup after add the sweet sorghum stalk stock quality of 30% ethanol than being 1:900～1100.
10. the method for a kind of sweet sorghum straw comprehensive utilization according to claim 1, is characterized in that, the Mierocrystalline cellulose making in above-mentioned steps (6) adopts cellulose degraded, then ferments, production of cellulosic ethanol.
The method of 11. a kind of sweet sorghum straw comprehensive utilizations according to claim 1, it is characterized in that, rare syrup of squeezing out in above-mentioned steps (6), or replace dilute sulphuric acid for the step (4) of next batch, the mass ratio of sweet sorghum stalk slurry slag and rare syrup is 1:4～6.
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