CN103589761B - A kind of method utilizing wheat bran to prepare xylo-oligosaccharide and the product obtained by the method - Google Patents
A kind of method utilizing wheat bran to prepare xylo-oligosaccharide and the product obtained by the method Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing wheat bran to prepare xylo-oligosaccharide and the product adopting described method to obtain, the method comprise raw materials pretreatment, High-temperature Liquefaction, removing protein, washing, be hydrolyzed, the enzyme that goes out, the step such as decolouring and desalination.The XOS of the low xylan product of the present invention
2-4content reaches more than 51.4%, XOS
2-7content reaches more than 73.1%.The present invention is low, and xylan product quality reaches xylo-oligosaccharide Industry code requirements, simultaneously, method of the present invention uses powder processing byproduct wheat bran as the extraction raw material of xylo-oligosaccharide product, its production cost reduces greatly, realize the efficiency utilization of wheat bran, improve the utility value of wheat bran, therefore, there is good popularizing application prospect.
Description
[technical field]
The invention belongs to food processing byproducts technical field of comprehensive utilization.More specifically, the present invention relates to a kind of method utilizing wheat bran to prepare xylo-oligosaccharide, also relate to the product adopting described method to obtain.
[background technology]
Wheat in China gross annual output amount is about 100,000,000 tons, and wheat bran output is about 20% of wheat processing amount, annual wheat bran output more than 2,000 ten thousand tons.Rich cellulose and hemicellulose in wheat bran, the main component xylan of its hemicellulose, is the inexhaustible and renewable resources leaved for development of a class, can produces the functional food ingredient such as xylo-oligosaccharide, Xylitol with physiologically active through Biochemical method.
Xylo-oligosaccharide is a kind of with containing the wood sugar (C that contracts more
5h
8o
4)
nthe agricultural byproducts of (also known as hemicellulose, n is mean polymerisation degree, generally about 150) composition, if boll hull, maize peel stamen, bagasse, stalk etc. are raw material, adopt the oligose that xylanase hydrolysis prepares.The raw material of current domestic production xylo-oligosaccharide is mainly corn cob, Testa Tritici, and the hemicellulose level (29.98%) in Testa Tritici is only second to corn cob (33.47% ~ 36.68%), is the good source of xylooligosaccharides production substrate xylan.
In recent years, no matter in the world or at home, functional oligose is increasingly extensive as the important component part application of foodstuff additive.Along with the fast development of functional food, functional beverage, functional dairy products, the market capacity of functional sugar is also sharply being expanded.In numerous functional oligose, xylo-oligosaccharide is considered the functional oligose that propagation bifidus bacillus function is best, suppress the growth of pathogenic bacteria spoilage organism, purification enteron aisle effect the best.Due to the uniqueness had compared with other oligose, can be applicable to be not suitable for using in the food (or protective foods) of other oligose, particularly acid and need the food (or protective foods) carrying out pyroprocessing.Suntory Ltd. of Japan carries out xylo-oligosaccharide suitability for industrialized production in the world at first.China also to set up the project the research carried out xylo-oligosaccharide suitability for industrialized production in the enforcement period of the ninth five-year plan.Shandong Longli Biology Science and Technology Co., Ltd and China Agricultural University's joint research and development develop the Industrialized processing technique of xylo-oligosaccharide, in the national science and technology assessment of result that April calendar year 2001 is organized by the Ministry of Education, have filled up domestic blank.Along with xylo-oligosaccharide is constantly recognized by consumers, many producers and R&D institution also put in the suitability for industrialized production of xylo-oligosaccharide one after another.By the end of the year 2010, domestic have six or seven newly-increased xylooligosaccharides production enterprises at least.Purity be 70% xylo-oligosaccharide internal price be about 160 yuan/kg, estimate that domestic xylo-oligosaccharide annual requirement is no less than 20,000 tons.
Abroad, xylo-oligosaccharide is succeeded in developing by Japanese Suntory company, and by Production by Enzymes, listing in 1989, when annual production 150 tons; 1998 yearly capacities reach 1100 tons (wherein 1000 tons, syrup, pressed powders 100 tons), syrup xylo-oligosaccharide content more than 70%, price about 2500 yen/kg, powder xylo-oligosaccharide content more than 95%, about 8000 yen/kg.Nearly 2 years, in Japan for the annual requirement of xylo-oligosaccharide and raffinose etc. at 10 ~ 200,000 tons.World market to the annual requirement of xylo-oligosaccharide with 25% speed increase.On the other hand, most leading enterprise develops functional foodstuff, has consolidated market.Other documents have also set forth the widespread popularity of functional low polyxylose and the diversity of raw material.About current trend, due to the reduction of production cost and the accreditation of human consumer make xylo-oligosaccharide industry will sustainable growth.New opportunities and challenges are created in this field with the xylo-oligosaccharide product food of Production by Enzymes.
The present invention utilizes the by product Testa Tritici in Flour production process to be raw material, by pre-treatment, the starch and albumen sepn that affect xylan extraction in Testa Tritici are removed, obtain the xylan crude extract that hemicellulose level is higher, recycling xylanase hydrolysis prepares functional low polyxylose, and the xylo-bioses-Xylotetrose content in product with physiologically active reaches more than 50%.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of method utilizing wheat bran to prepare xylo-oligosaccharide.
Another object of the present invention is to provide the xylo-oligosaccharide adopting described preparation method to prepare.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of method utilizing wheat bran to prepare xylo-oligosaccharide.
The step of the method is as follows:
A, raw materials pretreatment
100 ~ 300 weight part bran feedstock are crushed to 20 ~ 60 orders, add water in the bran powder obtained, make its concentration reach by weight 4% ~ 8%; Then use colloidal mill circular treatment 8 ~ 12min, obtain a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of wheat bran liquid steps A obtained is adjusted to 5.5 ~ 6.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with the enzyme work of described wheat bran liquid weighing scale 0.2 ~ 1.0 ‰ be 100000U/g: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in Jet liquefier under the condition of temperature 100 ~ 110 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 60 ~ 120min in popular response container under the condition of temperature 94 ~ 98 DEG C, so obtain a kind of liquefier; Described liquefier filters, and the filter cake obtained washes with water again;
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4% ~ 8%, again pH value is adjusted to 9.0 ~ 11.0, adjust the temperature to 45 ~ 55 DEG C, then the Sumizyme MP that to add with the work of described filter cake dry weight basis 0.5 ~ 1.5% enzyme be 200000U/g, continue reaction 2 ~ 4h, albumen is transformed into polypeptide or amino acid; Then filter with plate-and-frame filter press, the filter cake water washing of 8 ~ 12 times of displaced volumes;
D, washing
The washing leaching cake obtained toward step e adds 92 ~ 98% aqueous ethanolic solutions, its concentration is made to reach by weight 4% ~ 8%, then immersion 1 ~ 3h is stirred, filter with plate-and-frame filter press again, reclaim ethanol simultaneously, the filter cake the obtained water washing of 8 ~ 12 times of displaced volumes, obtain a kind of xylan, it re-uses twin-screw extruder and carry out High Temperature High Pressure extrusion process under the condition of temperature 140 DEG C ~ 160 DEG C, screw speed 40 ~ 80r/min, loading frequency 0.6 ~ 1.2 and pressure 6 ~ 10MPa, obtains a kind of pressing materials;
E, hydrolysis
In the pressing materials that step D obtains, add water, stirring and dissolving, make its concentration reach by weight 4% ~ 8%, again pH value is adjusted to 4.5 ~ 5.5, adjust the temperature to 48 ~ 52 DEG C, the zytase that to add with pressing materials dry weight basis 1 ~ 6 ‰ enzyme work be 5000U/g, be hydrolyzed reaction 12 ~ 24h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 100 ~ 105 DEG C of enzyme 1 ~ 3min that go out, and then filters with plate-and-frame filter press and obtains the thick liquid of xylo-oligosaccharide, be then concentrated into concentration by weight 30% ~ 40% with Three-effect concentration device;
G, decolouring
The pH value of concentrated solution step F obtained is adjusted to 3.5 ~ 4.5, temperature is adjusted to 70 ~ 80 DEG C, then solid weight meter 0.5 ~ 2.5% gac with concentrated solution is added, carry out decoloring reaction 20 ~ 40min, then filter, adopt supermicro filtration membrane to filter again and remove assorted sugar, obtain a kind of xylo-oligosaccharide liquid;
H, desalination
The xylo-oligosaccharide liquid allowing step G obtain, through ion-exchange chromatography, is removed the ion wherein contained, is obtained the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then described xylo-oligosaccharide liquid is concentrated into concentration by weight 70 ~ 80%, obtains described xylo-oligosaccharide product.
A preferred embodiment of the invention, in step, controls the temperature of the bran feedstock in process of lapping below 50 DEG C, to prevent the starch pasting in wheat bran.
According to another kind of preferred implementation of the present invention, in stepb, the condition of High-temperature Liquefaction is as follows: the pH value 5.8 ~ 6.2 of wheat bran liquid, α-amylase consumption are with described wheat bran liquid weighing scale 0.14 ~ 0.16 ‰, steam ejection liquefaction temperature 104 ~ 106 DEG C; Adding α-amylase consumption is with described wheat bran liquid weighing scale 0.28 ~ 0.32 ‰, gelatinization point 95 ~ 97 DEG C, gelatinization reaction times 60 ~ 120min.
According to another kind of preferred implementation of the present invention, in stepb, the temperature of described filter cake wash water is 85 ~ 90 DEG C.
According to another kind of preferred implementation of the present invention, in step C, the pH value of wheat bran slurries is adjusted to 9.5 ~ 10.5, temperature 48 ~ 52 DEG C, basic protein enzyme dosage are with described filter cake dry weight basis 0.8 ~ 1.2%, reaction times 2.8 ~ 3.2h.
According to another kind of preferred implementation of the present invention, in step C and step D, the temperature of described filter cake wash water is 50 ~ 60 DEG C.
According to another kind of preferred implementation of the present invention, in step D, under the condition of temperature 148 DEG C ~ 152 DEG C, screw speed 55 ~ 65r/min, loading frequency 0.8 ~ 1.0 and pressure 7.5 ~ 8.5MPa, carry out High Temperature High Pressure extrusion process, the water-content of described pressing materials is with described pressing materials total weight 40% ~ 46%.
According to another kind of preferred implementation of the present invention, in step e, described hydrolysis reaction condition is as follows: pH value 4.8 ~ 5.2, temperature 49 ~ 51 DEG C, zytase addition are with pressing materials dry weight basis 2 ~ 4 ‰, hydrolysis time 16 ~ 20h.
According to another kind of preferred implementation of the present invention, in step G, use the transmittance >60% of the xylo-oligosaccharide liquid of activated carbon decolorizing; The aperture of described supermicro filtration membrane is 600 ~ 1500D.
The invention still further relates to the xylo-oligosaccharide adopting described method to obtain, with described xylo-oligosaccharide total weight, XOS-70 type: XOS
2-7content>=73.1%, XOS
2-4content>=51.4%; Transmittance 72.5-78.4%, pH value 4.5-4.7 and ash content 0.19 ~ 0.24%.。
In more detail the present invention will be described below.
The present invention relates to a kind of method that wheat bran prepares xylo-oligosaccharide.
The described step preparing xylo-oligosaccharide method is as follows:
A, raw materials pretreatment
100 ~ 300 weight part bran feedstock are crushed to 20 ~ 60 orders, add water in the bran powder obtained, make its concentration reach by weight 4% ~ 8%; Then use colloidal mill circular treatment 8 ~ 12min, obtain a kind of wheat bran liquid;
In the present invention, described bran feedstock needs to carry out screening and pulverization process.Described screening is exactly the foreign matter existed in its bran feedstock, foreign material sieve are elected.Generally speaking, first can examine some larger foreign matter, foreign material by hand, then use the sieve of different size to sieve the foreign matter, the foreign material that go some less.
In the present invention, described bran feedstock adopts dry method to pulverize, and the effect of wet pulverization does not reach the requirement of the present invention to granularity far away.
Preferably, the concentration of wheat bran slurry is by weight 5% ~ 7%.More preferably, the concentration of wheat bran slurry is 5.5% ~ 6.5%.
In this step, the temperature of the bran feedstock in process of lapping is strict controlled in less than 50 DEG C, is conducive to the starch pasting prevented in wheat bran like this.
The pulverizer that the present invention uses is the disintegrating apparatus sold in the market, such as Jiangsu MuYang Group, Ltd., Shanghai Sai Shan powder machinery Manufacturing Co., Ltd, Jiangyin Hai Bang Machinery Manufacturing Co., Ltd. product sold.
The colloidal mill that the present invention uses is the disintegrating apparatus sold in the market, such as Wenzhou City's Changhong light equipment company limited, seven-star dairy equipment factory of Wenzhou City, Henan colloidal mill factory etc.
B, High-temperature Liquefaction
The pH value of wheat bran liquid steps A obtained is adjusted to 5.5 ~ 6.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with the enzyme work of described wheat bran liquid weighing scale 0.2 ~ 1.0 ‰ be 100000U/g: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in Jet liquefier under the condition of temperature 100 ~ 110 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 60 ~ 120min in popular response container under the condition of temperature 94 ~ 98 DEG C, so obtain a kind of liquefier; Described liquefier filters, and the filter cake obtained washes with water again.
The pH value of the wheat bran liquid using mineral acid regulating step A to obtain, described mineral acid is such as sulfuric acid, hydrochloric acid etc.The concentration of described mineral acid is generally 0.5 ~ 2.0N.
The High-temperature Liquefaction enzyme that the present invention uses is a kind of alpha-amylase, and its enzyme work is different because manufacturer is different.It is sold in the market, such as by Novozymes Company with product solds such as trade(brand)name liquozymeX.The High-temperature Liquefaction enzyme enzyme work that the present invention uses is 100000 ~ 120000.Its enzyme activity unit is U/g.
In the present invention, if the usage quantity of High-temperature Liquefaction enzyme is less than 0.2 ‰, then wheat bran starch liquefacation can be insufficient, and therefore starch can not become dextrin completely; If the usage quantity of High-temperature Liquefaction enzyme is greater than 1.0 ‰, then starch doubly can be cut into the less dextrin of molecular weight, is unfavorable for follow-up Mashing process; Therefore, the usage quantity of High-temperature Liquefaction enzyme is 0.2 ~ 1.0 ‰ is suitable, preferably 0.3 ~ 0.8 ‰, more preferably 0.4 ~ 0.6 ‰.In the present invention, it is to prevent the loss that in high-temperature injection liquefaction process, part enzyme is lived that α-amylase adds at twice, and then can affect overall liquefaction effect, and follow-up secondary adds the effect that α-amylase then can ensure to liquefy.
The Jet liquefier used when High-temperature Liquefaction process is the equipment sold in the market, such as by Shanghai Xiao Ledong tide company with trade(brand)name water heater, Wang Zhaoguang company with product solds such as trade(brand)name Jet liquefiers.
Preferably, in this step, the condition of High-temperature Liquefaction is as follows: the pH value 5.8 ~ 6.2 of wheat bran liquid, for the first time steam ejection liquefaction temperature 104 ~ 106 DEG C; Second time gelatinization point 95 ~ 97 DEG C, gelatinization reaction times 60 ~ 120min.
In this step, it is normally used plate-and-frame filter press in current chemical field that described liquefier filters the equipment used, the product solds such as such as Shandong Jing Jin filter press equipment company, Hangzhou emerging source plate frame filtering equipment company, Hangzhou Bei Te filter press equipment company.The feed pressure of described plate-and-frame filter press controls usually to control at 75 ~ 85 DEG C at 0.4 ~ 1.0MPa, filtration temperature usually.Filtering the filter cake obtained is carry out washing with the water that temperature is 85 ~ 90 DEG C.Wash water consumption (by volume) is 8 ~ 12 times of described sheet frame displaced volume, preferably 9 ~ 11 times, more preferably 9.5 ~ 10.5 times.The leaching requirement that the present invention uses is comparatively large, and the materials such as the dextrin produced after starch liquefacation are mainly removed, to improve the purity of object product by its object as far as possible.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4% ~ 8%, again pH value is adjusted to 9.0 ~ 11.0, adjust the temperature to 45 ~ 55 DEG C, then the Sumizyme MP that to add with the work of described filter cake dry weight basis 0.5 ~ 1.5% enzyme be 200000U/g, continue reaction 2 ~ 4h, albumen is transformed into polypeptide or amino acid; Then filter with plate-and-frame filter press, the filter cake water washing of 8 ~ 12 times of displaced volumes.
Sumizyme MP is that a kind of 2709 Bacillus subtilus microorganisms cultivated through bacterial protoplast mutafacient system are by submerged fermentation, extraction and refining proteolytic ferment, belong to the crisp outer high alkaline proteases of a kind of Serine, it can generate polypeptide or amino acid by hydrolyze protein molecules peptide chain, has the ability of stronger decomposing protein.The present invention uses the best results of Sumizyme MP, and the reaction times is short, and enzymolysis speed is high; Sumizyme MP price is lower in addition.The Sumizyme MP that the present invention uses is the commercial enzyme sold in the market, such as product sold such as Novi's letter (China) zymin company, Jie Nengke zymin company etc.The present invention uses the work of Sumizyme MP enzyme to be 180000 ~ 200000.Its enzyme activity unit is U/g.
In this step, preferably, the pH value of wheat bran slurries is adjusted to 9.5 ~ 10.5, temperature 48 ~ 52 DEG C, basic protein enzyme dosage be with described filter cake dry weight basis 0.8 ~ 1.2%, reaction times 2.8 ~ 3.2h.More preferably, the pH value of wheat bran slurries is adjusted to 9.9 ~ 10.0, temperature 49.5 ~ 50.5 DEG C, basic protein enzyme dosage be with described filter cake dry weight basis 0.9 ~ 1.1%, reaction times 2.8 ~ 3.2h.
In this step, filtering the plate-and-frame filter press used is normally used plate-and-frame filter press in current chemical field, the product solds such as such as Shandong Jing Jin filter press equipment company, Hangzhou emerging source plate frame filtering equipment company, Hangzhou Bei Te filter press equipment company.The feed pressure of described plate-and-frame filter press controls usually to control at 50 ~ 60 DEG C at 0.4 ~ 1.0MPa, filtration temperature usually.Filtering the filter cake obtained is carry out washing with the water that temperature is 50 ~ 60 DEG C.Wash water consumption (by volume) is 8 ~ 12 times of described sheet frame displaced volume, preferably 9 ~ 11 times, more preferably 9.5 ~ 10.5 times.
D, washing
The washing leaching cake obtained toward step e adds 92 ~ 98% aqueous ethanolic solutions, its concentration is made to reach by weight 4% ~ 8%, then immersion 1 ~ 3h is stirred, filter with plate-and-frame filter press again, reclaim ethanol simultaneously, the filter cake the obtained water washing of 8 ~ 12 times of displaced volumes, obtain a kind of xylan, it re-uses twin-screw extruder and carry out High Temperature High Pressure extrusion process under the condition of temperature 140 DEG C ~ 160 DEG C, screw speed 40 ~ 80r/min, loading frequency 0.6 ~ 1.2 and pressure 6 ~ 10MPa, obtains a kind of pressing materials.
The present invention uses aqueous ethanolic solution to wash as solvent, to remove some water-insoluble impurity, and such as a small amount of polysaccharide, part prolamine etc.
Preferably, described filter cake concentration is 5% ~ 7%, stirs soak time 1.5 ~ 2.5h; More preferably, described filter cake concentration is 5.5% ~ 6.5%, stirs soak time 1.8 ~ 2.2h.
The plate-and-frame filter press used carries out the operational condition of filtering as described by step C with using plate-and-frame filter press, does not repeat them here.
The present invention uses twin-screw extruder process xylan, and mainly because xylan is fiber substance, quality is tight, only have and it is broken up as much as possible, the efficiency of substrate and enzyme reaction could be increased, improve enzyme reaction effect, and extrusion operation energy consumption is lower relative to other processing modes.
The extrusion machine that the present invention uses is the equipment sold in the market, the twin-screw extruder such as sold by power & light company of the U.S., extrusion equipment by Jiangsu MuYang Group, Ltd., the rich equine Company in Hunan.
In this step, preferably, under the condition of temperature 144 DEG C ~ 156 DEG C, screw speed 50 ~ 70r/min, loading frequency 0.7 ~ 1.1 and pressure 7.0 ~ 8.0MPa, carry out High Temperature High Pressure extrusion process, the water-content of described pressing materials is with described pressing materials total weight 42% ~ 48%.。
More preferably, under the condition of temperature 148 DEG C ~ 152 DEG C, screw speed 55 ~ 65r/min, loading frequency 0.8 ~ 1.0 and pressure 7.5 ~ 8.5MPa, carry out High Temperature High Pressure extrusion process, the water-content of described pressing materials is with described pressing materials total weight 40% ~ 46%.
E, hydrolysis
In the pressing materials that step D obtains, add water, stirring and dissolving, make its concentration reach by weight 4% ~ 8%, again pH value is adjusted to 4.5 ~ 5.5, adjust the temperature to 48 ~ 52 DEG C, the zytase that to add with pressing materials dry weight basis 1 ~ 6 ‰ enzyme work be 5000U/g, be hydrolyzed reaction 12 ~ 24h.
Zytase is the enzyme adopting the techniques such as liquid submerged fermentation, ultrafiltration and spraying dry obtained.The xylan degrading contained in wheat bran can be become the xylo-oligosaccharide of specific size by the zytase that the present invention uses, i.e. final purpose product.The zytase that the present invention uses is product sold in the market, such as the product of Novi's letter zymin company, Jie Nengke zymin company, the grand large zymin Company in Shandong.The present invention uses xylanase activity to be 5000, and its enzyme activity unit is U/g.
In the present invention, the amount of zytase is the very important factor affecting its whole processing method.If the xylan enzyme amount of adding is less than 1 ‰, then the reaction times is long, affects the production cycle; If the xylan enzyme amount of adding is higher than 6 ‰, then the reaction times improves not obvious, increases production cost; Therefore, the amount of zytase is 1 ~ 6 ‰ is suitable.
Preferably, be hydrolyzed reaction times 15 ~ 21h under the condition of pH value 4.7 ~ 5.3, temperature 49 ~ 51 DEG C, zytase addition 2.5 ‰ ~ 3.5 ‰.More preferably, be hydrolyzed reaction times 17 ~ 19h under the condition of pH value 4.9 ~ 5.1, temperature 49.5 ~ 50.5 DEG C, zytase addition 2.8 ~ 3.2 ‰.
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 100 ~ 105 DEG C of enzyme 1 ~ 3min that go out, and then filters with plate-and-frame filter press and obtains the thick liquid of xylo-oligosaccharide, be then concentrated into concentration by weight 30% ~ 40% with Three-effect concentration device.
The object of enzyme of going out mainly controls the degree of enzyme reaction, controls the quality of the finished product.The functional effect of the such as xylo-oligosaccharide of conjugation between 2-4 is best, therefore must the effect of desmoenzyme and processing parameter, strict control enzyme dosage and reaction times, and need the instantaneous state by reaction system to fix at particular point in time, therefore the high temperature enzyme that goes out fast is a kind of conventional method.If can not go out enzyme in time, so part enzyme still can act on substrate, by 3 of part sugar, 4 sugar degradeds, thus can add the content of monose, cause product defective.
Preferably, the described enzyme that goes out carries out 1.5-2.5min under the condition of temperature 101-104 DEG C.More preferably, the described enzyme that goes out carries out 1.8-2.2min under the condition of temperature 102-103 DEG C.
The plate-and-frame filter press used in this step and the operational condition using plate-and-frame filter press to carry out filtering, as described by step C, do not repeat them here.
The Three-effect concentration device that the present invention uses is a kind of thickening equipment, and it is the thickening equipment sold in the market, such as, by product solds such as Yixing Grant thickening equipment company, Shanghai Rui Pai equipment company, Jiangsu Ke Wei equipment companies.
When thick for described xylo-oligosaccharide liquid being concentrated into concentration less than 30% with Three-effect concentration device is concentrated, then can concentration too low, be unfavorable for that follow-up workshop section implements, if when thick for described xylo-oligosaccharide liquid is concentrated into concentration more than 40%, then can excessive concentration, increase energy consumption, material viscosity increases simultaneously, follow-up decoloration process is difficult to carry out, and therefore, to select xylo-oligosaccharide thick liquid to concentrate concentration be 30% ~ 40% is appropriate.
G, decolouring
The pH value of concentrated solution step F obtained is adjusted to 3.5 ~ 4.5, temperature is adjusted to 70 ~ 80 DEG C, then solid weight meter 0.5 ~ 2.5% gac with concentrated solution is added, carry out decoloring reaction 20 ~ 40min, then filter, adopt supermicro filtration membrane to filter again and remove assorted sugar, obtain a kind of xylo-oligosaccharide liquid.
The pH value of the concentrated solution that step F obtains uses mineral acid to regulate, and described mineral acid is such as sulfuric acid, hydrochloric acid, nitric acid or phosphoric acid etc.Adjust ph use mineral acid concentration crucial especially, usual working concentration 0.5 ~ 2.0N mineral acid.
Gac is black powder or granular decolorizing carbon.Gac structurally because of microcrystalline carbon irregular alignment, forms pore between cross connection, and therefore, it is a kind of porous carbon, and tap density is low, and specific surface area is large.
Preferably, the concentrated solution that obtains of step F pH value 3.7-4.3, temperature 72-78 DEG C, carry out decoloring reaction under the condition of amounts of activated carbon 1.2-1.8%.
More preferably, the concentrated solution that obtains of step F pH value 3.9-4.1, temperature 74-76 DEG C, carry out decoloring reaction under the condition of amounts of activated carbon 1.4-1.6%.
The present invention uses granularity 200-400 order, the bulk density 0.4-0.45g/cm of gac
3.
The gac that the present invention uses is the gac of foodstuffs industry, the gac that such as Liyang City Zhong Yuan gac company, Pingquan County Hong De gac factory etc. sell.
Its medium wavelength of GB/T20885-2007(is adopted to select 420nm) detect, at the transmittance > 60% of the concentrated solution with activated carbon decolorizing.
The concentrated solution that step F obtains is needing to filter after decoloring reaction.The filter that the present invention uses is a kind of candle filter, is the filter plant sold in the market, such as the equipment of Yixing City lean Machinery Co., Ltd., Chengdu Xin Ming filter plant company limited and Yixing Chang Hua filter plant Company.
Filter the filtrate obtained also to need to carry out the assorted sugar of hyperfiltration removing.The supermicro filtration membrane that the present invention uses is a kind of organic polymer film, and the aperture of described supermicro filtration membrane is 600 ~ 1500D.
The ultra micro membrane filter plant that the present invention uses is a kind of equipment sold in the market, and such as Suntar (Xiamen) Environmental Engineering Co., Ltd., Chengdu link the product solds such as Influent Corp..
Obtain xylo-oligosaccharide liquid xylo-oligosaccharide content adopt QBT2984-2008 detect: XOS-70 type, XOS
2-7content>=73.1%(is in butt), XOS
2-4content>=51.4%(is in butt).
XOS
2-7content=[A
2× F
1+ (A
3+ A
4+ A
5+ A
6+ A
7) × F
2] × c × V × 100/ (A × m × 1000)
XOS
2-4content=[A
2× F
1+ (A
3+ A
4) × F
2] × c × V × 100/ (A × m × 1000)
XOS
2-7xylo-oligosaccharide (xylo-bioses-wood seven sugar) in-sample, %;
XOS
2-4xylo-oligosaccharide (xylo-bioses-Xylotetrose) in-sample, %;
A
2the peak area of xylo-bioses in-sample chromatogram figure;
A
3the peak area of xylotriose in-sample chromatogram figure;
A
4the peak area of Xylotetrose in-sample chromatogram figure;
A
5the peak area of wooden pentasaccharides in-sample chromatogram figure;
A
6the peak area of wooden six sugar in-sample chromatogram figure;
A
7the peak area of wooden seven sugar in-sample chromatogram figure;
Wood sugar peak area in xylose standard color atlas;
C-xylose standard strength of solution, unit is milligram every milliliter (mg/ml);
F1-using the reduction factor 0.93 of wood sugar as 1, XOS2;
F2-using the reduction factor 0.94 of wood sugar as 1, more than XOS3;
The quality (in butt) of m-sample, unit is gram (g);
The volume of V-sample, unit is milliliter (ml).
H, desalination
The xylo-oligosaccharide liquid allowing step G obtain, through ion-exchange chromatography, is removed the ion wherein contained, is obtained the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then described xylo-oligosaccharide liquid is concentrated into concentration by weight 70 ~ 80%, obtains described xylo-oligosaccharide product.
Ion exchange chromatography is a kind of method utilizing ion exchange principle and liquid chromatography technology separation solution cationic and negatively charged ion.The stationary phase of ion-exchange chromatography is generally ion exchange resin, there is many active centre that can ionize in resinous molecular structure, can there is ion-exchange with these active centre in the ion in component to be separated, form ion-exchange equilibrium, thus form distribution between moving phase and stationary phase.Mutually fight for the ion-exchange sites in stationary phase between ion in the intrinsic ion of stationary phase and component to be separated, and move along with the motion of moving phase, finally realize separation
The ion exchange resin that the present invention uses is the combination of strong acidic ion resin and strongly basic anionic resin.The ion-exchange chromatography that the present invention uses is product sold in the market, and such as French Novasep, million photo bio engineering corporation product solds, use its ion-exchange chromatography according to institute's sell goods specification sheets.
The xylo-oligosaccharide liquid that step G obtains needs to concentrate after ion-exchange chromatography process.In the present invention, the concentrated equipment used is quadruple effect thickener, and it is product sold in the market, the product solds such as such as Yixing Grant thickening equipment company, Shanghai Rui Pai equipment company, Jiangsu Ke Wei equipment company.
The concentrated xylo-oligosaccharide product obtained carries out its content detection according to QBT2984-2008.With described xylo-oligosaccharide total weight, XOS-70 type: XOS
2-7content>=73.1%, XOS
2-4content>=51.4%; Transmittance 72.5-78.4%, pH value 4.5-4.7 and ash content 0.19 ~ 0.24%.
The xylo-oligosaccharide adopting the inventive method to prepare can be used as the foodstuff additive of the various food sold in the market as functional oligose.
The method that the present invention utilizes wheat bran to prepare xylo-oligosaccharide has following feature:
1, adopt impurity removal method to remove the impurity such as starch, albumen, improve the content of substrate xylo-oligosaccharide, be convenient to the carrying out of xylo-oligosaccharide hydrolysis reaction, raise the efficiency.
2, adopt twin-screw extruder to carry out high temperature high pressure process to the xylo-oligosaccharide after purifying, achieved the preliminary cracking of xylo-oligosaccharide by physical method, improve follow-up enzyme digestion reaction efficiency.
3, adopt up-to-date membrane technique to be separated assorted sugar, improve the purity of object product oligomeric wood sugar.
[beneficial effect]
The invention has the beneficial effects as follows: starch, albumen, fat and polysaccharide that the present invention adopts enzymolysis process removal flour processing by product wheat bran to contain, and the xylan orientation of its wheat bran is changed into xylo-oligosaccharide, the XOS of the low xylan product of the present invention
2-4content reaches more than 51.4%, XOS
2-7content reaches more than 73.1%, reaches the requirement of GBT2948-2008 xylo-oligosaccharide product index.
The present invention is low, and xylan product quality reaches xylo-oligosaccharide Industry code requirements, simultaneously, method of the present invention uses powder processing byproduct wheat bran as the extraction raw material of xylo-oligosaccharide product, its production cost reduces greatly, realize the efficiency utilization of wheat bran, improve the utility value of wheat bran, therefore, there is good popularizing application prospect.
[embodiment]
The present invention can be understood better by following embodiment.
Embodiment 1: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.100 weight part bran feedstock are crushed to 60 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Jiangsu MuYang Group, Ltd. to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 5.5%; Then the colloidal mill circular treatment 10min using Changhong light equipment company limited of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 0.5N sulfuric acid steps A to be obtained is adjusted to 6.0, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.2 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name water heater by the damp company of Shanghai Xiao Ledong under the condition of temperature 104 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 80min in popular response container under the condition of temperature 96 DEG C, so obtain a kind of liquefier; Described liquefier uses the plate-and-frame filter press sold by Shandong Jing Jin filter press equipment company to filter under the condition of 0.6MPa, filtration temperature 78 DEG C, and the filter cake obtained washs with the water of temperature 86 DEG C again; Wash water consumption (by volume) is 8 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 8%, again pH value is adjusted to 9.0, adjust the temperature to 48 DEG C, then add and believe that the enzyme of (China) zymin Company is lived as the Sumizyme MP of 200000U/g with described filter cake dry weight basis 0.5% by Novi, continue reaction 2.0h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 94% aqueous ethanolic solution, its concentration is made to reach by weight 5.5%, then stir and soak 1.8h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses the twin-screw extruder sold by Jiangsu MuYang Group, Ltd. temperature 140 DEG C, screw speed 40r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 0.6 and the condition of pressure 6.0MPa, obtaining a kind of water-content is with described pressing materials total weight 44% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 6%, again pH value is adjusted to 4.5, adjust the temperature to 48 DEG C, add and believe by Novi the zytase that the enzyme work of zymin Company is 5000U/g with pressing materials dry weight basis 1.0 ‰, be hydrolyzed reaction 12h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 100 DEG C of enzyme 1.0min that go out, then use the filtration of identical with step C plate-and-frame filter press to obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 34 by the Three-effect concentration device of Yixing Grant thickening equipment Company;
G, decolouring
The pH value of the concentrated solution using 0.5N sulfuric acid mineral acid step F to be obtained is adjusted to 3.5, temperature is adjusted to 70 DEG C, then add with the gac of the solid weight meter 0.5% of concentrated solution by gac Company far away in Liyang City, carry out decoloring reaction 30min, then the filter sold by Yixing City lean Machinery Co., Ltd. is used to filter, adopt the supermicro filtration membrane (aperture 1200D) sold by Suntar (Xiamen) Environmental Engineering Co., Ltd. to filter again and remove assorted sugar, obtain a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 71.29%, XOS
2-4content is 50.35%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by French Novasep, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use by the quadruple effect thickener of Yixing Grant thickening equipment Company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 75%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 73.48%, XOS
2-4content is 51.38%, transmittance 75.50%, pH value 4.60, and ash content 0.24% reaches the requirement of XOS-70 type product.
Embodiment 2: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.240 weight part bran feedstock are crushed to 20 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 4.0%; Then the colloidal mill circular treatment 9min using seven-star dairy equipment factory of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 0.8N hydrochloric acid steps A to be obtained is adjusted to 6.2, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 1.0 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: add the described High-temperature Liquefaction enzyme of about 1/3rd for the first time, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name Jet liquefier by Wang Zhaoguang company under the condition of temperature 106 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 100min in popular response container under the condition of temperature 94 DEG C, so obtain a kind of liquefier; Described liquefier uses the plate-and-frame filter press of Hangzhou emerging source plate frame filtering equipment Company to filter under the condition of 0.4MPa, filtration temperature 80 DEG C, and the filter cake obtained washs with the water of temperature 88 DEG C again; Wash water consumption (by volume) is 12 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4%, again pH value is adjusted to 11.0, adjust the temperature to 52 DEG C, then the Sumizyme MP that to add with described filter cake dry weight basis 0.9% be 200000U/g by the enzyme work of Jie Neng section zymin Company, continue reaction 2.8h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 92% aqueous ethanolic solution, its concentration is made to reach by weight 6.5%, then stir and soak 2.2h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses by the twin-screw extruder of the rich equine Company in Hunan temperature 160 DEG C, screw speed 80r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 1.2 and the condition of pressure 10MPa, obtaining a kind of water-content is with described pressing materials total weight 40% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 8%, again pH value is adjusted to 5.5, adjust the temperature to 52 DEG C, add the zytase being 5000U/g by the enzyme work of Jie Neng section zymin Company with pressing materials dry weight basis 6.0 ‰, be hydrolyzed reaction 24h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 105 DEG C of enzyme 3.0min that go out, then use the plate-and-frame filter press identical with step C to filter and obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 30% by the Three-effect concentration device of Shanghai Rui Pai equipment company sale;
G, decolouring
The pH value of the concentrated solution using 1.0N hydrochloric acid mineral acid step F to be obtained is adjusted to 4.5, temperature is adjusted to 80 DEG C, then add with the gac of the solid weight meter 2.5% of concentrated solution by gac Company far away in Liyang City, carry out decoloring reaction 26min, then the filter sold by Chengdu Xin Ming filter plant company limited is used to filter, the supermicro filtration membrane (aperture 800D) adopting Chengdu to link Influent Corp.'s sale again filters removes assorted sugar, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 73.65%, XOS
2-4content is 52.83%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by million photo bio engineering corporatioies, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use the quadruple effect thickener sold by Shanghai Rui Pai equipment company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 78%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 74.96%, XOS
2-4content is 53.55%, transmittance 74.50%, pH value 4.50, and ash content 0.22% reaches the requirement of XOS-70 type product.
Embodiment 3: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.Use the disintegrating apparatus sold by Jiangyin Hai Bang Machinery Manufacturing Co., Ltd., 120 weight part bran feedstock are crushed to 40 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran.Add water in the bran powder obtained, stir, make its concentration reach by weight 6.5%; Then the colloidal mill circular treatment 8min using Henan colloidal mill factory to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 1.2N nitric acid steps A to be obtained is adjusted to 5.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.3 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name water heater by the damp company of Shanghai Xiao Ledong under the condition of temperature 100 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 60min in popular response container under the condition of temperature 96 DEG C, so obtain a kind of liquefier; Described liquefier uses the plate-and-frame filter press sold by Hangzhou Bei Te filter press equipment company to filter under the condition of 0.6MPa, filtration temperature 75 DEG C, and the filter cake obtained washs with the water of temperature 85 DEG C again; Wash water consumption (by volume) is 9 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 6%, again pH value is adjusted to 9.5, adjust the temperature to 45.0 DEG C, then add and believe that the enzyme of (China) zymin Company is lived as the Sumizyme MP of 200000U/g with described filter cake dry weight basis 1.1% by Novi, continue reaction 3.2h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 94% aqueous ethanolic solution, its concentration is made to reach by weight 4.0%, then stir and soak 1.0h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses the twin-screw extruder sold by Jiangsu MuYang Group, Ltd. temperature 144 DEG C, screw speed 50r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 0.7 and the condition of pressure 7.0MPa, obtaining a kind of water-content is with described pressing materials total weight 42% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 8, again pH value is adjusted to 4.7, adjust the temperature to 49.0 DEG C, add the zytase being 5000U/g by the enzyme work of the grand large zymin Company in Shandong with pressing materials dry weight basis 2.5 ‰, be hydrolyzed reaction 15h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 101 DEG C of enzyme 1.5min that go out, then use the plate-and-frame filter press identical with step C to filter and obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 32% by the Three-effect concentration device of Jiangsu Ke Wei equipment company sale;
G, decolouring
The pH value of the concentrated solution using 1.5N sulfuric acid mineral acid step F to be obtained is adjusted to 3.7, temperature is adjusted to 72 DEG C, then the gac sold by Pingquan County Hong De gac factory with the solid weight meter 1.2% of concentrated solution is added, carry out decoloring reaction 20min, then use and filtered by the filter of Yixing Chang Hua filter plant Company, the supermicro filtration membrane (aperture 1000D) adopting Suntar (Xiamen) Environmental Engineering Co., Ltd. to sell again filters removes assorted sugar, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 72.50%, XOS
2-4content is 51.29%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by million photo bio engineering corporatioies, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use the quadruple effect thickener sold by Jiangsu Ke Wei equipment company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 70%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 73.10%, XOS
2-4content is 51.86%, transmittance 78.35%, pH value 4.60, and ash content 0.22% reaches the requirement of XOS-70 type product.
Embodiment 4: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.300 weight part bran feedstock are crushed to 20 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Jiangsu MuYang Group, Ltd. to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 7.0%; Then the colloidal mill circular treatment 10min using Changhong light equipment company limited of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 1.6N sulfuric acid steps A to be obtained is adjusted to 5.8, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.8 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name water heater by the damp company of Shanghai Xiao Ledong under the condition of temperature 110 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 80min in popular response container under the condition of temperature 98 DEG C, so obtain a kind of liquefier; The plate-and-frame filter press that described liquefier uses Shandong Jing Jin filter press equipment company to sell filters under the condition of 0.8MPa, filtration temperature 82 DEG C, and the filter cake obtained washs with the water of temperature 86 DEG C again; Wash water consumption (by volume) is 11 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4%, again pH value is adjusted to 10.5, adjust the temperature to 55.0 DEG C, then add and believe that the enzyme of (China) zymin Company is lived as the Sumizyme MP of 200000U/g with described filter cake dry weight basis 1.5% by Novi, continue reaction 4.0h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 96% aqueous ethanolic solution, its concentration is made to reach by weight 8.0%, then stir and soak 1.5h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses by the twin-screw extruder of the rich equine Company in Hunan temperature 156 DEG C, screw speed 70r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 1.1 and the condition of pressure 8.0MPa, obtaining a kind of water-content is with described pressing materials total weight 44% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 4%, again pH value is adjusted to 5.3, adjust the temperature to 51 DEG C, add and believe by Novi the zytase that the enzyme work of zymin Company is 5000U/g with pressing materials dry weight basis 3.5 ‰, be hydrolyzed reaction 21h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 104 DEG C of enzyme 2.5min that go out, then use the filtration of identical with step C plate-and-frame filter press to obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 36% by the Three-effect concentration device of Yixing Grant thickening equipment Company;
G, decolouring
Use 0.5N sulfuric acid mineral acid, the pH value of concentrated solution step F obtained is adjusted to 4.3, temperature is adjusted to 78 DEG C, then the gac sold by Pingquan County Hong De gac factory with the solid weight meter 1.8% of concentrated solution is added, carry out decoloring reaction 34min, then the filter using Yixing City lean Machinery Co., Ltd. to sell filters, then the supermicro filtration membrane (aperture 600D) adopting Chengdu to link Influent Corp.'s sale filters the assorted sugar of removal, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 73.50%, XOS
2-4content is 52.25%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by million photo bio engineering corporatioies, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use by the quadruple effect thickener of Yixing Grant thickening equipment Company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 72%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 75.04%, XOS
2-4content is 53.87%, transmittance 76.55%, pH value 4.65, and ash content 0.20% reaches the requirement of XOS-70 type product.
Embodiment 5: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.160 weight part bran feedstock are crushed to 40 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 5.0%; Then the colloidal mill circular treatment 12min using Changhong light equipment company limited of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 1.8N sulfuric acid steps A to be obtained is adjusted to 6.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.4 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name water heater by the damp company of Shanghai Xiao Ledong under the condition of temperature 108 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 100min in popular response container under the condition of temperature 94 DEG C, so obtain a kind of liquefier; Described liquefier uses the plate-and-frame filter press of Hangzhou emerging source plate frame filtering equipment Company to filter under the condition of 1.0MPa, filtration temperature 85 DEG C, and the filter cake obtained washs with the water of temperature 88 DEG C again; Wash water consumption (by volume) is 9.5 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 6%, again pH value is adjusted to 9.9, adjust the temperature to 49.5 DEG C, then the Sumizyme MP that to add with described filter cake dry weight basis 0.8% be 200000U/g by the enzyme work of Jie Neng section zymin Company, continue reaction 2.8h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 98% aqueous ethanolic solution, its concentration is made to reach by weight 5%, then stir and soak 2.5h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses by the twin-screw extruder of the rich equine Company in Hunan temperature 148 DEG C, screw speed 55r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 0.8 and the condition of pressure 7.5MPa, obtaining a kind of water-content is with described pressing materials total weight 46% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 6%, again pH value is adjusted to 4.9, adjust the temperature to 49.5 DEG C, add the zytase being 5000U/g by the enzyme work of the grand large zymin Company in Shandong with pressing materials dry weight basis 2.8 ‰, be hydrolyzed reaction 17h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 102 DEG C of enzyme 1.8min that go out, then use the plate-and-frame filter press identical with step C to filter and obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 40% by the Three-effect concentration device of Jiangsu Ke Wei equipment company sale;
G, decolouring
The pH value of the concentrated solution using 0.8N sulfuric acid mineral acid step F to be obtained is adjusted to 3.9, temperature is adjusted to 74 DEG C, then add with the gac of the solid weight meter 1.4% of concentrated solution by gac Company far away in Liyang City, carry out decoloring reaction 40min, then the filter of Yixing Chang Hua filter plant Company is used to filter, the supermicro filtration membrane (aperture 1400D) adopting Suntar (Xiamen) Environmental Engineering Co., Ltd. to sell again filters removes assorted sugar, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 72.30%, XOS
2-4content is 51.28%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by French Novasep, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use by the quadruple effect thickener of Yixing Grant thickening equipment Company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 80%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 73.75%, XOS
2-4content is 52.53%, transmittance 72.50%, pH value 4.50, and ash content 0.23% reaches the requirement of XOS-70 type product.
Embodiment 6: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.200 weight part bran feedstock are crushed to 60 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Jiangsu MuYang Group, Ltd. to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 8%; Then the colloidal mill circular treatment 10min using seven-star dairy equipment factory of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 2.0N vitriol acid+nitric acid steps A to be obtained is adjusted to 6.0, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.6 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: first time add about 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name water heater by the damp company of Shanghai Xiao Ledong under the condition of temperature 106 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 120min in popular response container under the condition of temperature 98 DEG C, so obtain a kind of liquefier; The plate-and-frame filter press that described liquefier uses Hangzhou Bei Te filter press equipment company to sell filters under the condition of 0.8MPa, filtration temperature 78 DEG C, and the filter cake obtained washs with the water of temperature 90 DEG C again; Wash water consumption (by volume) is 10.5 times of described sheet frame displaced volume;
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 8%, again pH value is adjusted to 10.0, adjust the temperature to 50.5 DEG C, then add and believe that the enzyme of (China) zymin Company is lived as the Sumizyme MP of 200000U/g with described filter cake dry weight basis 1.2% by Novi, continue reaction 3.2h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 96% aqueous ethanolic solution, its concentration is made to reach by weight 7%, then stir and soak 3h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses the twin-screw extruder sold by Jiangsu MuYang Group, Ltd. temperature 152 DEG C, screw speed 65r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 1.0 and the condition of pressure 8.5MPa, obtaining a kind of water-content is with described pressing materials total weight 42% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 8%, again pH value is adjusted to 5.1, adjust the temperature to 50.5 DEG C, add the zytase being 5000U/g by the enzyme work of Jie Neng section zymin Company with pressing materials dry weight basis 3.2 ‰, be hydrolyzed reaction 19h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 103 DEG C of enzyme 2.2min that go out, then use the filtration of identical with step C plate-and-frame filter press to obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 38% by the Three-effect concentration device of Yixing Grant thickening equipment Company;
G, decolouring
Use 0.5N sulfuric acid mineral acid, the pH value of concentrated solution step F obtained is adjusted to 4.1, temperature is adjusted to 76 DEG C, then add with the gac of the solid weight meter 1.6% of concentrated solution by gac Company far away in Liyang City, carry out decoloring reaction 30min, then the filter using Chengdu Xin Ming filter plant company limited to sell filters, then the supermicro filtration membrane (aperture 1500D) adopting Chengdu to link Influent Corp.'s sale filters the assorted sugar of removal, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 72.86%, XOS
2-4content is 52.03%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by million photo bio engineering corporatioies, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use the quadruple effect thickener sold by Jiangsu Ke Wei equipment company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 75%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 73.74%, XOS
2-4content is 52.86%, transmittance 74.58%, pH value 4.53, and ash content 0.21% reaches the requirement of XOS-70 type product.
Embodiment 7: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.240 weight part bran feedstock are crushed to 40 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Jiangsu MuYang Group, Ltd. to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 7%; Then the colloidal mill circular treatment 12min using Henan colloidal mill factory to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 2.0N sulfuric acid steps A to be obtained is adjusted to 6.0, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 1.0 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: add the described High-temperature Liquefaction enzyme of about 1/3rd for the first time, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name Jet liquefier by Wang Zhaoguang company under the condition of temperature 100 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 100min in popular response container under the condition of temperature 98 DEG C, so obtain a kind of liquefier; Described liquefier uses the plate-and-frame filter press of Hangzhou emerging source plate frame filtering equipment Company to filter under the condition of 0.8MPa, filtration temperature 78 DEG C, and the filter cake obtained washs with the water of temperature 88 DEG C again; Wash water consumption (by volume) is 9 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4%, again pH value is adjusted to 9.9, adjust the temperature to 50.5 DEG C, then the Sumizyme MP that to add with described filter cake dry weight basis 0.5% be 200000U/g by the enzyme work of Jie Neng section zymin Company, continue reaction 2.8h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 96% aqueous ethanolic solution, its concentration is made to reach by weight 5%, then stir and soak 3h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses by the twin-screw extruder of the rich equine Company in Hunan temperature 140 DEG C, screw speed 80r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 0.7 and the condition of pressure 7.5MPa, obtaining a kind of water-content is with described pressing materials total weight 42% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 6%, again pH value is adjusted to 5.5, adjust the temperature to 49 DEG C, add the zytase being 5000U/g by the enzyme work of the grand large zymin Company in Shandong with pressing materials dry weight basis 3.5 ‰, be hydrolyzed reaction 21h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 102 DEG C of enzyme 2.2min that go out, then use the filtration of identical with step C plate-and-frame filter press to obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 40% by the Three-effect concentration device of Yixing Grant thickening equipment Company;
G, decolouring
Use 0.5N sulfuric acid mineral acid, the pH value of concentrated solution step F obtained is adjusted to 4.5, temperature is adjusted to 72 DEG C, then the gac sold by Pingquan County Hong De gac factory with the solid weight meter 1.8% of concentrated solution is added, carry out decoloring reaction 40min, then the filter using Chengdu Xin Ming filter plant company limited to sell filters, then the supermicro filtration membrane (aperture 1400D) adopting Chengdu to link Influent Corp.'s sale filters the assorted sugar of removal, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 73.59%, XOS
2-4content is 52.18%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by million photo bio engineering corporatioies, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use the quadruple effect thickener sold by Shanghai Rui Pai equipment company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 75%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 74.95%, XOS
2-4content is 53.73%, transmittance 75.13%, pH value 4.60, and ash content 0.19% reaches the requirement of XOS-70 type product.
Embodiment 8: adopt the inventive method to prepare xylo-oligosaccharide
The implementation step of this embodiment is as follows:
A, raw materials pretreatment
Sieve is used the foreign matter existed in its bran feedstock, foreign material sieve to be elected.300 weight part bran feedstock are crushed to 40 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran by the disintegrating apparatus using Shanghai Sai Shan powder machinery Manufacturing Co., Ltd to sell.Add water in the bran powder obtained, stir, make its concentration reach by weight 8%; Then the colloidal mill circular treatment 10min using Changhong light equipment company limited of Wenzhou City to sell, obtains a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of the wheat bran liquid using 0.8N sulfuric acid steps A to be obtained is adjusted to 5.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with described wheat bran liquid weighing scale 0.4 ‰ be 100000U/g by Novozymes Company with the enzyme work that trade(brand)name liquozymeX sells: add the described High-temperature Liquefaction enzyme of about 1/3rd for the first time, described wheat bran liquid carries out high temperature gelatinization in the Jet liquefier sold with trade(brand)name Jet liquefier by Wang Zhaoguang company under the condition of temperature 108 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 80min in popular response container under the condition of temperature 98 DEG C, so obtain a kind of liquefier; The plate-and-frame filter press that described liquefier uses Shandong Jing Jin filter press equipment company to sell filters under the condition of 0.6MPa, filtration temperature 80 DEG C, and the filter cake obtained washs with the water of temperature 85 DEG C again; Wash water consumption (by volume) is 11 times of described sheet frame displaced volume.
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 6%, again pH value is adjusted to 10.0, adjust the temperature to 48 DEG C, then the Sumizyme MP that to add with the work of described filter cake dry weight basis 0.9% enzyme be 200000U/g, continue reaction 3.2h, albumen is transformed into polypeptide or amino acid; Then use plate-and-frame filter press to filter, filter cake washes with water, and its filtration condition and wash conditions are as identical in step D's;
D, washing
The washing leaching cake obtained toward step e adds 96% aqueous ethanolic solution, its concentration is made to reach by weight 5%, then stir and soak 3h, re-using the plate-and-frame filter press identical with step C under the condition identical with step C filters, reclaim ethanol simultaneously, the filter cake obtained washs under using the condition identical with step C, obtain a kind of xylan, it re-uses by the twin-screw extruder of the rich equine Company in Hunan temperature 140 DEG C, screw speed 80r/min, High Temperature High Pressure extrusion process is carried out under loading frequency 0.7 and the condition of pressure 7.5MPa, obtaining a kind of water-content is with described pressing materials total weight 46% pressing materials,
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 6%, again pH value is adjusted to 5.5, adjust the temperature to 49 DEG C, add and believe by Novi the zytase that the enzyme work of zymin Company is 5000U/g with pressing materials dry weight basis 3.5 ‰, be hydrolyzed reaction 17h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 102 DEG C of enzyme 2.2min that go out, then use the filtration of identical with step C plate-and-frame filter press to obtain the thick liquid of xylo-oligosaccharide, then use and be concentrated into concentration by weight 38% by the Three-effect concentration device of Yixing Grant thickening equipment Company;
G, decolouring
The pH value of the concentrated solution using 1.5N nitric acid mineral acid step F to be obtained is adjusted to 4.5, temperature is adjusted to 72 DEG C, then add with the gac of the solid weight meter 1.8% of concentrated solution by gac Company far away in Liyang City, carry out decoloring reaction 30min, then the filter using Chengdu Xin Ming filter plant company limited to sell filters, the supermicro filtration membrane (aperture 1400D) adopting Suntar (Xiamen) Environmental Engineering Co., Ltd. to sell again filters removes assorted sugar, obtains a kind of xylo-oligosaccharide liquid;
Detect according to QBT2984-2008 xylo-oligosaccharide industry standard, obtain XOS
2-7content is 73.86%, XOS
2-4content is 52.36%.
H, desalination
The ion-exchange chromatography of the xylo-oligosaccharide liquid allowing step G obtain through being sold by French Novasep, removes the ion wherein contained, obtains the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then use by the quadruple effect thickener of Yixing Grant thickening equipment Company, described xylo-oligosaccharide liquid is concentrated into concentration by weight 75%, obtains described xylo-oligosaccharide product.Its xylo-oligosaccharide content is detected, XOS according to QBT2984-2008
2-7content is 75.05%, XOS
2-4content is 54.17%, transmittance 76.37%, pH value 4.69, and ash content 0.19% reaches the requirement of XOS-70 type product.
Claims (8)
1. utilize wheat bran to prepare a method for xylo-oligosaccharide, it is characterized in that the step of the method is as follows:
A, raw materials pretreatment
100 ~ 300 weight part bran feedstock are ground to 20 ~ 60 orders, the temperature of the bran feedstock in process of lapping are controlled below 50 DEG C, to prevent the starch pasting in wheat bran; Add water in the bran powder obtained, make its concentration reach by weight 4% ~ 8%; Then use colloidal mill circular treatment 8 ~ 12min, obtain a kind of wheat bran liquid;
B, High-temperature Liquefaction
The pH value of wheat bran liquid steps A obtained is adjusted to 5.5 ~ 6.5, again at twice toward the High-temperature Liquefaction enzyme that wherein to add with the enzyme work of described wheat bran liquid weighing scale 0.2 ~ 1.0 ‰ be 100000U/g: first time add 1/3rd described High-temperature Liquefaction enzyme, described wheat bran liquid carries out high temperature gelatinization in Jet liquefier under the condition of temperature 100 ~ 110 DEG C; Then second time adds remaining High-temperature Liquefaction enzyme, and described wheat bran liquid carries out gelatinization reaction 60 ~ 120min in popular response container under the condition of temperature 94 ~ 98 DEG C, so obtain a kind of liquefier; Described liquefier filters, and the filter cake obtained is the water washing of 85 ~ 90 DEG C again by temperature;
C, removing protein
The washing leaching cake interpolation water obtained toward step B is sized mixing, its concentration is made to reach by weight 4% ~ 8%, again pH value is adjusted to 9.0 ~ 11.0, adjust the temperature to 45 ~ 55 DEG C, then the Sumizyme MP that to add with the work of described filter cake dry weight basis 0.5 ~ 1.5% enzyme be 200000U/g, continue reaction 2 ~ 4h, albumen is transformed into polypeptide or amino acid; Then filter with plate-and-frame filter press, the filter cake water washing of 8 ~ 12 times of displaced volumes;
D, washing
The washing leaching cake obtained toward step C adds 92 ~ 98% aqueous ethanolic solutions, its concentration is made to reach by weight 4% ~ 8%, then immersion 1 ~ 3h is stirred, filter with plate-and-frame filter press again, reclaim ethanol simultaneously, the filter cake the obtained water washing of 8 ~ 12 times of displaced volumes, obtain a kind of xylan, it re-uses twin-screw extruder and carry out High Temperature High Pressure extrusion process under the condition of temperature 140 DEG C ~ 160 DEG C, screw speed 40 ~ 80r/min, loading frequency 0.6 ~ 1.2 and pressure 6 ~ 10MPa, obtains a kind of pressing materials;
E, hydrolysis
Water is added in the pressing materials that step D obtains, stirring and dissolving, its concentration is made to reach by weight 4% ~ 8%, again pH value is adjusted to 4.5 ~ 5.5, adjust the temperature to 48 ~ 52 DEG C, add the zytase being 5000U/g with pressing materials dry weight basis 1 ~ 6 ‰ enzyme work, be hydrolyzed reaction 12 ~ 24h;
F, go out enzyme
The temperature of hydrolysis reaction liquid step e obtained is adjusted to 100 ~ 105 DEG C of enzyme 1 ~ 3min that go out, and then filters with plate-and-frame filter press and obtains the thick liquid of xylo-oligosaccharide, be then concentrated into concentration by weight 30% ~ 40% with Three-effect concentration device;
G, decolouring
The pH value of concentrated solution step F obtained is adjusted to 3.5 ~ 4.5, temperature is adjusted to 70 ~ 80 DEG C, then solid weight meter 0.5 ~ 2.5% gac with concentrated solution is added, carry out decoloring reaction 20 ~ 40min, then filter, adopt supermicro filtration membrane to filter again and remove assorted sugar, obtain a kind of xylo-oligosaccharide liquid;
H, desalination
The xylo-oligosaccharide liquid allowing step G obtain, through ion-exchange chromatography, is removed the ion wherein contained, is obtained the xylo-oligosaccharide liquid that specific conductivity is 15 below μ s/cm; Then described xylo-oligosaccharide liquid is concentrated into concentration by weight 70 ~ 80%, obtains described xylo-oligosaccharide product.
2. method according to claim 1, is characterized in that in stepb, and the condition of High-temperature Liquefaction is as follows: the pH value 5.8 ~ 6.2 of wheat bran liquid, α-amylase consumption are with described wheat bran liquid weighing scale 0.14 ~ 0.16 ‰, steam ejection liquefaction temperature 104 ~ 106 DEG C; Adding α-amylase consumption is with described wheat bran liquid weighing scale 0.28 ~ 0.32 ‰, gelatinization point 95 ~ 97 DEG C, gelatinization reaction times 60 ~ 120min.
3. method according to claim 1, is characterized in that in step C, and the pH value of wheat bran slurries is adjusted to 9.5 ~ 10.5, temperature 48 ~ 52 DEG C, Sumizyme MP alkalescence consumption are with described filter cake dry weight basis 0.8 ~ 1.2%, reaction times 2.8 ~ 3.2h.
4. method according to claim 1, is characterized in that in step C and step D, and the temperature of described filter cake wash water is 50 ~ 60 DEG C.
5. method according to claim 1, it is characterized in that in step D, under the condition of temperature 148 DEG C ~ 152 DEG C, screw speed 55 ~ 65r/min, loading frequency 0.8 ~ 1.0 and pressure 7.5 ~ 8.5MPa, carry out High Temperature High Pressure extrusion process, the water-content of described pressing materials is with described pressing materials total weight 40% ~ 46%.
6. method according to claim 1, is characterized in that in step e, and described hydrolysis reaction condition is as follows: pH value 4.8 ~ 5.2, temperature 49 ~ 51 DEG C, zytase addition are with pressing materials dry weight basis 2 ~ 4 ‰, hydrolysis time 16 ~ 20h.
7. method according to claim 1, is characterized in that in step G, uses the transmittance >60% of the xylo-oligosaccharide liquid of activated carbon decolorizing; The aperture of described supermicro filtration membrane is 600 ~ 1500D.
8. the xylo-oligosaccharide that method obtains according to claim 1-7, is characterized in that with described xylo-oligosaccharide total weight, XOS-70 type: XOS
2-7content>=73.1%, XOS
2-4content>=51.4%; Transmittance 72.5-78.4%, pH value 4.5-4.7 and ash content 0.19 ~ 0.24%.
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| CN108486194B (en) * | 2018-03-22 | 2021-07-13 | 吉林省农业科学院 | Method for preparing solid fruit glucose from corn flour |
| CN110938662A (en) * | 2019-12-12 | 2020-03-31 | 青岛科海生物有限公司 | Production method for improving itaconic acid yield by using bran |
| CN111004827B (en) * | 2019-12-27 | 2021-09-03 | 山东百龙创园生物科技股份有限公司 | Preparation method of xylo-oligosaccharide |
| CN112301077A (en) * | 2020-11-09 | 2021-02-02 | 安阳市豫鑫木糖醇科技有限公司 | Method for producing xylooligosaccharide by continuous liquefaction coupling enzyme method of hemicellulose powder |
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| CN1333371A (en) * | 2000-07-07 | 2002-01-30 | 无锡轻工大学 | Enzymatic preparation of high-purity xylo-oligosaccharide |
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| CN1333371A (en) * | 2000-07-07 | 2002-01-30 | 无锡轻工大学 | Enzymatic preparation of high-purity xylo-oligosaccharide |
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