CN104341233A - Method for high-efficiency extraction of nutrient substances in undaria pinnatifida sporophyll - Google Patents
Method for high-efficiency extraction of nutrient substances in undaria pinnatifida sporophyll Download PDFInfo
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- CN104341233A CN104341233A CN201310341401.9A CN201310341401A CN104341233A CN 104341233 A CN104341233 A CN 104341233A CN 201310341401 A CN201310341401 A CN 201310341401A CN 104341233 A CN104341233 A CN 104341233A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a method for high-efficiency extraction of nutrient substances in undaria pinnatifida sporophyll, and is characterized in that the method comprises the following steps: (1) raw material pretreatment, (2) ultrasonic treatment, (3) cellulose enzymolysis, (4) proteolysis, (5) brine digestion, (6) dilution and filtration, (7) decoloring, (8) CaCl2 solution treatment, (9) ion exchange, (10) preparation of sodium alginate, (11) preparation of ethanol, and (12) preparation of an undaria pinnatifida sporophyll organic fertilizer. A composite enzyme is prepared from protease, pectinase and cellulase by a scientific ratio, and raw material is pretreated, so as to improve the extraction rate of sodium alginate; at the same time, fuel ethanol is prepared by using cellulose-rich undaria pinnatifida sporophyll processing waste; Chinese humic acid resources are fully developed and utilized in the processing process, the organic fertilizer rich in humic acid and macronutrients is produced with water as a solvent, and the high-valued comprehensive utilization of the undaria pinnatifida sporophyll is realized.
Description
Technical field
The present invention relates to Undaria pinnatifida Suringar and utilize field, be specifically related to a kind of method of high efficiency extraction Undaria pinnatifida Suringar Middle nutrition material.
Background technology
Our times is faced with the immense pressure of energy shortage and environmental pollution, and the renewable energy source that exploitation is cleaned has become the important means solving fossil resources and energy dilemma.Bio-ethanol is subject to extensive concern as a kind of clean fuel and gasoline dope.At present, China prepares alcohol fuel and mainly lays particular emphasis on the Lu Yuan raw materials such as stalk, bagasse, wood chip and cassava, but it is less to prepare the research of bio-ethanol to Living marine resources, the technical study backwardness relatively in the exploitation of Undaria pinnatifida Suringar biomass energy.
Ocean area is huge, the Undaria pinnatifida Suringar that is richly stored with resource, and it is of a great variety, photosynthetic efficiency is high, growth cycle is short, and the biomass total amount produced by photosynthesis every year just reaches 550x10
8ton is a kind of huge renewable resources, is also the potential resources producing biomass energy.The Undaria pinnatifida Suringar processing waste of rich cellulose, Undaria pinnatifida Suringar polysaccharide, N.F,USP MANNITOL is utilized to prepare alcohol fuel, Undaria pinnatifida Suringar processing waste not only can be made to turn waste into wealth, solve problem of environmental pollution, also can be the raw material supply prepared bio-ethanol and provide sufficient and cheap, promote the technological development of the marine biomass energy.
Sodium alginate, a kind of natural polysaccharide, has the stability needed for pharmaceutical preparation auxiliary material, solvability, viscosity and security.1881, first Englishize scholar E.C.Stanford carried out scientific research to the Undaria pinnatifida Suringar hydrochlorate extract in brown Undaria pinnatifida Suringar.He finds that this alignic extract has several very interesting characteristic, and it has concentrated solution, forms the ability of gel and film forming.Based on this, he proposes the application of several suitability for industrialized production.But Undaria pinnatifida Suringar hydrochlorate is until 50 years just carry out large-scale industrial production.Commercially produce and start from nineteen twenty-seven, the present whole world about produces 30000 tons every year, and wherein 30% for foodstuffs industry, and remaining is industrial for other, pharmacy industry and dentistry.
It is ripe not enough that current zymohydrolysis extracting method extracts sodium alginate, often all just have employed single cellulase to be hydrolyzed, but composition plant cell wall has the compositions such as cellulase, hemicellulase, pectin, xylogen, on-link mode (OLM) between them or inlay, or obvolvent, so be difficult to single enzyme the cell walls thoroughly cracking plant, content can not be made to discharge completely.
Humic acids is animals and plants remains, mainly the plant remains natural polymer organic compound of element of the first species's complexity that formed and accumulate through the decomposition of microorganism and conversion and a series of process of geochemistry, and it exists with entity indeed.Terrestrial plant was had to start a large amount of accumulation before about 400,000,000 years.Large surprising of humic-acid-type substances quantity, number is with trillion tons of calculating.Peat, brown coal, the hundreds billion of ton of weathered coal of humic-acid-type substances are rich in China, extremely abundant.Resource of humic acid big country, no matter humic acids science and technology and application are depth & wideths, all not too adapt to the needs of national economic development and ecological construction, also have no small gap compared with some developed country's level.The potential advantages of humic acids do not play.
How thoroughly to crack the cell walls of plant, content is discharged completely.Avoid again being subject to other people's molecular substance, as the interference of pectin, protein etc., the present invention considers to make prozyme with proteolytic enzyme, polygalacturonase, cellulase by the proportioning of science, pre-treatment is carried out to raw material, and then extract on the basis of sodium alginate, make full use of Undaria pinnatifida Suringar raw material production ethanol.By adding the compositions such as potassium primary phosphate, xanthohumic acid, urea, sodium nitrophenolate, fully to develop the resource of humic acid of China, produce the fertilizer being rich in humic acids.
Summary of the invention
For solving the technical barrier existed in above-mentioned technology, the invention provides a kind of method of high efficiency extraction Undaria pinnatifida Suringar nutritive substance, it is characterized in that, described method comprises the steps:
(1) raw materials pretreatment: Undaria pinnatifida Suringar raw material is removed silt, dry to below moisture content 8-10% in 60-70 DEG C, being crushed to grain graininess is that the powder of below 1.0-1.5mm is as raw material;
(2) supersound process: the water adding 40-60 times of weight in powder, with 400-600W ultrasonication 15-20min;
(3) fiber enzymolysis: adjust pH to be 4-6 with 4-8mol/L hydrochloric acid, add the cellulase 0.4-0.6% be made up of inscribe β-dextranase 40%, circumscribed β-dextranase 35%, β-glucose lucerne enzyme 25% of raw material weight 0.5-2.0%, enzymolysis 3-4 hour at 50-60 DEG C;
(4) proteolysis: add the proteinase-10 .3-0.4% be made up of neutral protease 55%, papoid 45%, the polygalacturonase 0.2-0.3% be made up of pectin lyase 50%, Rohapect MPE 50%, continues enzymolysis 4-5h, stirs, centrifugation after enzymolysis;
(5) salt solution digestion: to above-mentioned centrifugal after Undaria pinnatifida Suringar in add the 2-3% Na of 13-15 times of Undaria pinnatifida Suringar weight
2cO
3solution, digests 2-3h in 55-65 DEG C of water-bath;
(6) dilute filtration: the fresh tap water then adding volume 5-7 times 55-65 DEG C carries out dilution 1.5-2h, fully after dilution evenly, is filtered by 280-350 object tulle;
(7) decolour: filtrate adds the hydrogen peroxide of 0.2-0.3%, at 55-60 DEG C of decolouring 1-2h, be then warmed up to 80-90 DEG C and keep 10-20min, filter with 280-350 object tulle;
(8) CaCl
2solution-treated: filtrate slowly adds the CaCl of volume ratio 2-3% concentration 10%
2solution, leaves standstill 1-2h, then filters, with CaCl residual in fresh tap water cleaning calcium alginate fiber
2solution and other impurity;
(9) ion-exchange: calcium alginate adds 13-15 purified water doubly, then by 1.5-2.5 doubly 10% NaCl solution, carries out ion-exchange, makes calcium alginate fiber be converted into sodium alginate solution completely in 50-60 DEG C of water-bath;
(10) sodium alginate processed: then use the alcohol precipitation of 95%, obtains sodium alginate, and sodium alginate obtains finished product through dehydration, oven dry, pulverizing;
(11) ethanol processed: the centrifugal filtrate autoclaving in step (4), after cooling, adds activated yeast, and inoculative proportion is 20-25%, 27-35 DEG C and seals and continue to cultivate fermentation in 4-8 days, and ethanol is produced in fermented liquid distillation;
(12) Undaria pinnatifida Suringar fertilizer processed: take sucrose 2-3kg stirring and dissolving in 20-25kg water, 0.5-0.6kg sodium nitrophenolate is added and 0.4-0.5kg Nafusaku makes it whole dissolving under stirring, to add after step (11) distillation ethanol in remaining liquid, take that xanthohumic acid 20-22kg pulverizes, urea 14-16kg and potassium primary phosphate 20-25kg mixes and adds above-mentioned mixed solution, namely the 30-35kg stirring and dissolving that simultaneously adds water obtains this liquid fertilizer.
The method of above-mentioned a kind of high efficiency extraction Undaria pinnatifida Suringar Middle nutrition material, is characterized in that: fermentative production of ethanol in described step (11), after enzymolysis solution sterilizing, accesses activated industrial yeast bacterial classification CICC31447, carries out fermentation culture.
The method of above-mentioned a kind of high efficiency extraction Undaria pinnatifida Suringar Middle nutrition material, is characterized in that: described step (11) fermentative production of ethanol, and enzymolysis solution is through the yeast of overactivation at 30 DEG C, and fermentation culture 7 days, the bio-ethanol amount obtained is maximum.
Beneficial effect of the present invention:
The present invention makes prozyme with proteolytic enzyme, polygalacturonase, cellulase by the proportioning of science, avoid being subject to other people's molecular substance, as the interference of pectin, protein etc., pre-treatment is carried out to raw material, thoroughly crack the cell walls of plant, the main components such as the Mierocrystalline cellulose in Undaria pinnatifida Suringar, protein are separated, and is converted into the available monose of microorganism, oligosaccharides and free protein, be conducive to the extraction yield improving sodium alginate; Utilize the Undaria pinnatifida Suringar processing waste of rich cellulose to prepare alcohol fuel simultaneously; In the course of processing, remaining waste liquid is by adding the compositions such as potassium primary phosphate, xanthohumic acid, urea, sodium nitrophenolate, and fully to develop the resource of humic acid of China, producing with water is solvent, is rich in the fertilizer of humic acids, macronutrient.Achieve the high-valued comprehensive utilization of Undaria pinnatifida Suringar, develop the marine organisms energy.
Embodiment
embodiment 1:
Undaria pinnatifida Suringar raw material is removed silt, and dry to moisture content less than 8% in 60 DEG C, being crushed to grain graininess is that the powder of below 1.0mm is as raw material; Accurately take and dry the 100kg Undaria pinnatifida Suringar after pulverizing, add the fresh tap water of raw material weight 4000ml, with 400W ultrasonication 15min; Adjust pH to be 4 with 4mol/L hydrochloric acid, to add at the cellulase 0.4%, 50 DEG C be made up of inscribe β-dextranase 40%, circumscribed β-dextranase 35%, β-glucose lucerne enzyme 25% of raw material weight 0.5% enzymolysis 3 hours; Add the proteinase-10 .3% be made up of neutral protease 55%, papoid 45%, the polygalacturonase 0.2% be made up of pectin lyase 50%, Rohapect MPE 50%, continue enzymolysis 4h, stir, centrifugation after enzymolysis;
To above-mentioned centrifugal after Undaria pinnatifida Suringar in add 1300kg 2% Na
2cO
3solution, digests 2h in 55 DEG C of water-baths; Then the fresh tap water adding volume 5 times 55 DEG C carries out dilution 1.5h, fully after dilution evenly, is filtered by 280 object tulles; Filtrate adds the hydrogen peroxide of 0.2%, at 55 DEG C of decolouring 1h, is then warmed up to 80 DEG C and keeps 10min, filter with 280 object tulles; Filtrate slowly adds the CaCl of volume ratio 2% concentration 10%
2solution, leaves standstill 1h, then filters, with CaCl residual in fresh tap water cleaning calcium alginate fiber
2solution and other impurity; Calcium alginate adds the purified water of 13 times, then uses 1.5 times of 10% NaCl solution, in 50 DEG C of water-baths, carries out ion-exchange, makes calcium alginate fiber be converted into sodium alginate solution completely; Then use the alcohol precipitation of 95%, obtain sodium alginate, sodium alginate obtains finished product 28.3 grams through dehydration, oven dry, pulverizing.
First industrial yeast is placed in nutrient solution and cultivates activation, medium component is 1% yeast extract paste, 2% peptone, 2% glucose, above raw material is dissolved in water, in 121 DEG C of sterilizing 15min, then inoculate in clean operator's console, cultivate 1 day, by pretreated for Undaria pinnatifida Suringar enzymolysis solution autoclaving, after cooling for 30 DEG C, add activated yeast, inoculative proportion is 10%, 28 DEG C and seals and continue cultivation fermentation in 3 days, and ethanol is produced in fermented liquid distillation, after cultivation terminates, the alcohol concn measured wherein is about 3.5%, after distillation, obtains bio-ethanol.
Take sucrose 2kg stirring and dissolving in 20kg water, 0.5kg sodium nitrophenolate is added and 0.4kg Nafusaku makes it whole dissolving under stirring, to add after distillation ethanol in remaining liquid, take that xanthohumic acid 20kg pulverizes, urea 14kg and potassium primary phosphate 20kg mixes and adds above-mentioned mixed solution, namely the 30kg stirring and dissolving that simultaneously adds water obtains this liquid fertilizer, then spray is dry, pulverize, make Undaria pinnatifida Suringar fertilizer, the content of the N P and K in fertilizer is about 42%, and the content of total organic matter is 62%.
embodiment 2:
Undaria pinnatifida Suringar raw material is removed silt, and dry to moisture content less than 10% in 70 DEG C, being crushed to grain graininess is that the powder of below 1.5mm is as raw material; Accurately take and dry the 100kg Undaria pinnatifida Suringar after pulverizing, add the fresh tap water of raw material weight 4000ml, with 600W ultrasonication 20min; Adjust pH to be 6 with 8mol/L hydrochloric acid, to add at the cellulase 0.6%, 60 DEG C be made up of inscribe β-dextranase 40%, circumscribed β-dextranase 35%, β-glucose lucerne enzyme 25% of raw material weight 2.0% enzymolysis 4 hours; Add the proteinase-10 .4% be made up of neutral protease 55%, papoid 45%, the polygalacturonase 0.3% be made up of pectin lyase 50%, Rohapect MPE 50%, continue enzymolysis 5h, stir, centrifugation after enzymolysis;
To above-mentioned centrifugal after Undaria pinnatifida Suringar in add 1500kg 3% Na
2cO
3solution, digests 3h in 65 DEG C of water-baths; Then the fresh tap water adding volume 7 times 65 DEG C carries out dilution 2h, fully after dilution evenly, is filtered by 350 object tulles; Filtrate adds the hydrogen peroxide of 0.3%, at 60 DEG C of decolouring 2h, is then warmed up to 90 DEG C and keeps 20min, filter with 350 object tulles; Filtrate slowly adds the CaCl of volume ratio 3% concentration 10%
2solution, leaves standstill 2h, then filters, with CaCl residual in fresh tap water cleaning calcium alginate fiber
2solution and other impurity; Calcium alginate adds the purified water of 15 times, then uses 2.5 times of 10% NaCl solution, in 50-60 DEG C of water-bath, carries out ion-exchange, makes calcium alginate fiber be converted into sodium alginate solution completely; Then use the alcohol precipitation of 95%, obtain sodium alginate, sodium alginate obtains finished product 28.3 grams through dehydration, oven dry, pulverizing.
First industrial yeast is placed in nutrient solution and cultivates activation, medium component is 1% yeast extract paste, 2% peptone, 2% glucose, above raw material is dissolved in water, in 121 DEG C of sterilizing 15min, then inoculate in clean operator's console, cultivate 1 day, by pretreated for Undaria pinnatifida Suringar enzymolysis solution autoclaving, after cooling for 30 DEG C, add activated yeast, inoculative proportion is 10%, 28 DEG C and seals and continue cultivation fermentation in 3 days, and ethanol is produced in fermented liquid distillation, after cultivation terminates, the alcohol concn measured wherein is about 3.7%, after distillation, obtains bio-ethanol.
Take sucrose 3kg stirring and dissolving in 25kg water, 0.6kg sodium nitrophenolate is added and 0.5kg Nafusaku makes it whole dissolving under stirring, to add after distillation ethanol in remaining liquid, take that xanthohumic acid 22kg pulverizes, urea 16kg and potassium primary phosphate 25kg mixes and adds above-mentioned mixed solution, namely the 35kg stirring and dissolving that simultaneously adds water obtains this liquid fertilizer, then spray is dry, pulverize, make Undaria pinnatifida Suringar fertilizer, the content of the N P and K in fertilizer is about 55%, and the content of total organic matter is 61%.
Claims (3)
1. a method for high efficiency extraction Undaria pinnatifida Suringar nutritive substance, is characterized in that, described method comprises the steps:
(1) raw materials pretreatment: Undaria pinnatifida Suringar raw material is removed silt, dry to below moisture content 8-10% in 60-70 DEG C, being crushed to grain graininess is that the powder of below 1.0-1.5mm is as raw material;
(2) supersound process: the water adding 40-60 times of weight in powder, with 400-600W ultrasonication 15-20min;
(3) fiber enzymolysis: adjust pH to be 4-6 with 4-8mol/L hydrochloric acid, add the cellulase 0.4-0.6% be made up of inscribe β-dextranase 40%, circumscribed β-dextranase 35%, β-glucose lucerne enzyme 25% of raw material weight 0.5-2.0%, enzymolysis 3-4 hour at 50-60 DEG C;
(4) proteolysis: add the proteinase-10 .3-0.4% be made up of neutral protease 55%, papoid 45%, the polygalacturonase 0.2-0.3% be made up of pectin lyase 50%, Rohapect MPE 50%, continues enzymolysis 4-5h, stirs, centrifugation after enzymolysis;
(5) salt solution digestion: to above-mentioned centrifugal after Undaria pinnatifida Suringar in add the 2-3% Na of 13-15 times of Undaria pinnatifida Suringar weight
2cO
3solution, digests 2-3h in 55-65 DEG C of water-bath;
(6) dilute filtration: the fresh tap water then adding volume 5-7 times 55-65 DEG C carries out dilution 1.5-2h, fully after dilution evenly, is filtered by 280-350 object tulle;
(7) decolour: filtrate adds the hydrogen peroxide of 0.2-0.3%, at 55-60 DEG C of decolouring 1-2h, be then warmed up to 80-90 DEG C and keep 10-20min, filter with 280-350 object tulle;
(8) CaCl
2solution-treated: filtrate slowly adds the CaCl of volume ratio 2-3% concentration 10%
2solution, leaves standstill 1-2h, then filters, with CaCl residual in fresh tap water cleaning calcium alginate fiber
2solution and other impurity;
(9) ion-exchange: calcium alginate adds 13-15 purified water doubly, then by 1.5-2.5 doubly 10% NaCl solution, carries out ion-exchange, makes calcium alginate fiber be converted into sodium alginate solution completely in 50-60 DEG C of water-bath;
(10) sodium alginate processed: then use the alcohol precipitation of 95%, obtains sodium alginate, and sodium alginate obtains finished product through dehydration, oven dry, pulverizing;
(11) ethanol processed: the centrifugal filtrate autoclaving in step (4), after cooling, adds activated yeast, and inoculative proportion is 20-25%, 27-35 DEG C and seals and continue to cultivate fermentation in 4-8 days, and ethanol is produced in fermented liquid distillation;
(12) Undaria pinnatifida Suringar fertilizer processed: take sucrose 2-3kg stirring and dissolving in 20-25kg water, 0.5-0.6kg sodium nitrophenolate is added and 0.4-0.5kg Nafusaku makes it whole dissolving under stirring, to add after step (11) distillation ethanol in remaining liquid, take that xanthohumic acid 20-22kg pulverizes, urea 14-16kg and potassium primary phosphate 20-25kg mixes and adds above-mentioned mixed solution, namely the 30-35kg stirring and dissolving that simultaneously adds water obtains this liquid fertilizer.
2. the method for a kind of high efficiency extraction Undaria pinnatifida Suringar Middle nutrition material according to claim 1, it is characterized in that: fermentative production of ethanol in described step (11), after enzymolysis solution sterilizing, access activated industrial yeast bacterial classification CICC31447, carry out fermentation culture.
3. the method for a kind of high efficiency extraction Undaria pinnatifida Suringar Middle nutrition material according to claim 1, it is characterized in that: described step (11) fermentative production of ethanol, enzymolysis solution is through the yeast of overactivation at 30 DEG C, and fermentation culture 7 days, the bio-ethanol amount obtained is maximum.
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| CN105924283A (en) * | 2016-04-29 | 2016-09-07 | 武汉皓达农业科技有限公司 | Preparation method for colorless organic water-soluble fertilizer |
| CN107349240A (en) * | 2017-06-23 | 2017-11-17 | 百色学院 | A kind of extracting method of mangrove bark polyphenol |
| CN109020708A (en) * | 2018-09-18 | 2018-12-18 | 中国农业科学院农业环境与可持续发展研究所 | Itself a kind of sustained release alga fertilizer preparation method |
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