CN101705253A - Method for treating xylose mother solution - Google Patents
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Abstract
The invention relates to a method for treating xylose mother solution. The method comprises the following steps: firstly, using glucose in the alcohol yeast strain fermented xylose mother solution to prepare alcohol by distilling; and then, using xylose in the xylose yeast strain fermented mother solution to prepare xylitol by extracting, and finally extracting gum sugar. The method changes the xylose mother solution into valuable by using the two-step fermentation method, so on the one hand, the method reduces the inhibiting effect brought about by excessive glucose during producing the xylitol by fermenting, and on the other hand, improves the utilization rates of the glucose and the xylose mother solution, and greatly reduces the COD treated as wastewater at the same time; and the production process is simple, safe and energy-saving.
Description
Technical field
The present invention relates to technical field of biological fermentation, especially, the present invention relates to a kind of treatment process of xylose mother liquid.
Background technology
Wood sugar is a kind of important function derived food additives and sweeting agent, because of it has unique chemical character and physiological function, be specially adapted to patients' such as diabetes, obesity dietotherapy additive, the production method of Xylitol mainly is a chemical method at present, promptly adopt corn cob, bagasse etc. to be rich in the raw material of poly-pentose, become to contain the hydrolyzed solution of wood sugar through acidolysis, from hydrolyzed solution, extract wood sugar through neutralization, decolouring, ion-exchange, crystalline step then.
Xylose mother liquid is a kind of waste liquid of processing behind the wood sugar, contains abundant glucose, wood sugar, pectinose and semi-lactosi.Wherein wood sugar and pectinose all are five-carbon sugars, and difficulty is utilized by microorganism.At present, the Xylitol barms can utilize wood sugar wherein and be translated into Xylitol, if but directly utilize the substratum of xylose mother liquid as xylitol fermentation, the secondary metabolites that abundant glucose forms during the fermentation in the mother liquor can be converted into Xylitol by the severe inhibition wood sugar, make that fermentation sugar alcohol yield is on the low side, therefore must control the concentration of glucose in the xylitol fermentation substratum.
Utilize the main path of xylose mother liquid to have following several at present: 1, to utilize xylose mother liquid to produce wood sugar and Xylitol, the production process complexity, need separate other impurity such as wood sugar and pectinose, glucose and pectinose fail to make full use of in the xylose mother liquid simultaneously; 2, utilize xylose mother liquid to produce pectinose, the production process complexity need be for further processing to xylose mother liquid; 3, utilize xylose mother liquid to produce furfural, relate to high temperature, highly compressed synthesis condition.
The present invention is by the research to each composition in the xylose mother liquid, a kind of method that fully utilizes xylose mother liquid is proposed, can make full use of glucose abundant in the mother liquor on the one hand, on the other hand, also can make full use of wherein wood sugar, pectinose, not only improve the utilization ratio of xylose mother liquid greatly, and reduced the COD of xylose mother liquid, reduced the wastewater treatment difficulty.
Summary of the invention
The treatment process that the purpose of this invention is to provide a kind of xylose mother liquid.
The treatment process of xylose mother liquid of the present invention is to utilize two-step fermentation, utilizes distillery yeast bacterial classification fermentation glucose wherein to prepare alcohol earlier, distill alcohol; Utilize the wood sugar in the Xylitol barms fermentation mother liquor to prepare Xylitol then, fermented liquid successively extracts Xylitol and pectinose.
Specifically, may further comprise the steps:
1) with xylose mother liquid as carbon source, the configuration glucose concn be the alcoholic fermentation medium of 2～3% (m/v);
2) the distillery yeast bacterial classification is inoculated in the alcoholic fermentation medium cultivates, reduce to until glucose concn and stop fermentation below 0.3% (m/v);
3) fermentation liquid obtains alcohol through distillation, refilters to remove yeast and partial impurities;
4) filtrate and xylose mother liquid are mixed as carbon source, make that to contain glucose concn be 1.0～1.2% (m/v), and xylose concentration is the xylitol fermentation substratum of 10～15% (m/v);
5) the Xylitol barms is inoculated in the xylitol fermentation substratum cultivates; When being lower than 0.8% (m/v), finishes residual xylose concentration in the fermented liquid fermentation; Fermentation ends after-filtration fermented liquid is removed yeast and partial impurities, and filtrate is used for successively extracting Xylitol and pectinose.
Step 2) in, described cultivation is following to be carried out, and carries out aerobic earlier and cultivates, and feeds sterile air and stirring; Breed when yeast cell and stop logical sterile air when the OD value is 40～60, stream adds xylose mother liquid control glucose concn at 1～2% (m/v) simultaneously; When the fermentation liquid volume reaches 60～90% liquid amounts, stop stream and add, continue fermentation and reduce to below 0.3% (m/v) until glucose concn.
In the step 5), described cultivation is following to be carried out, and carries out aerobic earlier and cultivates, and feeds sterile air and stirring; Breed when the OD value is 20～30 when yeast cell, change little oxygen over to and cultivate.
It is to feed sterile air and stirring in the culturing process that described aerobic is cultivated, and the velocity ratio of described sterile air is 1: 0.4～1: 1.
Described micro-aerobe fermentation is to feed sterile air and stirring in the culturing process, and the velocity ratio of described sterile air is 1: 0.1～1: 0.3.
The distillery yeast bacterial classification that the present invention adopts can be this area and produces ethanol recombination microzyme or bacterium commonly used, as S.cerevisiae ZU-10; The Xylitol barms that the present invention adopts can be this area and produces Xylitol yeast or bacterium commonly used, as Candida sp.;
Step 2) and 5) culture temperature can determine that general zymamsis can be selected 26～32 ℃ for use according to concrete bacterial classification; Xylitol fermentation can be selected 24～32 ℃ for use; The inoculum size of bacterial classification is also determined according to common practise by those skilled in the art, generally can be selected from 1%～25%, preferred 5%～10%.
Preferably, in the step 5), described cultivation is following to be carried out, elder generation feeds sterile air with 1: 0.5 velocity ratio, mixing speed 300rpm, 28～31 ℃ are carried out aerobic and cultivate, and the velocity ratio feeding sterile air with 1: 0.3 changes little oxygen cultivation stage over to when OD value is 20～30 when yeast cell is bred.
Described fermention medium, comprise in described alcoholic fermentation medium and the described xylitol fermentation substratum, also comprise nitrogenous source and inorganic salt, used nitrogenous source is this area nitrogenous source commonly used, is preferably in yeast powder, peptone, corn steep liquor, the urea one or more; Used inorganic salt also adopt this area inorganic salt commonly used, as sal epsom, potassium primary phosphate etc.
Described filtration can be adopted this area filter method commonly used, as centrifugal, press filtration, vacuum filtration etc.
Step 3) and 5) yeast and the partial impurities that obtains after the filtration can be used for preparing feed.
Preferably, the treatment process of xylose mother liquid of the present invention may further comprise the steps:
1) with xylose mother liquid as carbon source, the configuration glucose concn be the alcoholic fermentation medium of 2～3% (m/v);
2) the distillery yeast bacterial classification is inoculated into carries out aerobic in the alcoholic fermentation medium and cultivate, feed sterile air and stirring, breed when yeast cell and to stop logical sterile air carry out zymamsis when the OD value is 40～60, stream adds xylose mother liquid control glucose concn at 1～2% (m/v) simultaneously; When the fermentation liquid volume reaches 60～90% liquid amounts, stop stream and add, continue fermentation and reduce to below 0.3% until glucose;
3) fermentation liquid obtains alcohol through distillation, refilters to remove yeast and partial impurities;
4) filtrate and xylose mother liquid are mixed as carbon source, make that to contain glucose concn be 1.0～1.2% (m/v), and xylose concentration is the xylitol fermentation substratum of 10～15% (m/v);
5) the Xylitol barms is inoculated into aerobic yeast culture in the xylitol fermentation substratum, when yeast cell is bred the micro-aerobe fermentation stage that changes over to when the OD value is 20～30; When being lower than 0.8% (m/v), finishes residual xylose concentration in the fermented liquid fermentation.Fermentation ends after-filtration fermented liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again.
Among the present invention, specialize as nothing, used per-cent is the quality volume percent.
The treatment process of xylose mother liquid of the present invention is to utilize the distillery yeast bacterial classification to remove glucose in the mother liquor, and the retarding effect that too much glucose brings when having reduced xylitol zymolysis production has on the one hand improved the utilization ratio of glucose on the other hand; Then the wood sugar in the xylose mother liquid is converted into Xylitol, through after extracting Xylitol and two kinds of high value added products of pectinose, COD reduces greatly in the former wood sugar mother liquor, not only xylose mother liquid is turned waste into wealth, and has reduced the processing costs of xylose mother liquid again; Production process is simple, safe, energy-conservation.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Specialize as nothing, distillery yeast bacterial classification that adopts among the embodiment and Xylitol barms are respectively gene engineering yeast (S.cerevisiae ZU-10) and candiyeast (Candidatropicalis), all available from Zhejiang University
Xylose mother liquid is to adopt acid technological process with corn cob hydrolysis under 115 ℃～125 ℃ conditions, through remaining processing-waste behind the extraction wood sugar.
Through Liquid Detection, the data of a certain batch of xylose mother liquid acquisition are glucose 14.57% (m/v), wood sugar 44.76% (m/v), pectinose 17.42% (m/v), semi-lactosi 11.63% (m/v).
Embodiment 1
The preparation alcoholic fermentation medium: xylose mother liquid 20% (m/v), yeast powder 0.5% (m/v), corn steep liquor 1.0% (m/v), potassium primary phosphate 0.05% (m/v), sal epsom 0.075% (m/v), tap water is settled to 1.08L, the pH nature.Adopt the 5L fermentor tank.
Alcoholic fermentation medium 110 ℃ of sterilizations 15 minutes, is inserted the cultured gene engineering yeast liquid seeds of 0.12L (S.cerevisiae ZU-10) when being cooled to 30 ℃.Feed sterile air with 1: 0.6 velocity ratio, mixing speed 300rpm, cultivated about 9 hours for 30 ℃, cell concn optical density(OD) (O.D.) value is 40.3, stops ventilation, keep mixing speed, continue to cultivate, culture temperature is increased to 33 ℃, and the mode that adds xylose mother liquid by stream is controlled the glucose concn of fermention medium in 1～2% (m/v) scope, when the fermentation liquid volume reaches 3.5L, stop stream and add xylose mother liquid, continue to be cultured to fermentation ends.
Adopt gas chromatography determination, ethanol concn reaches 4.76% (v/v) in the fermented liquid, and fermentation period 78 hours, sugar alcohol transformation efficiency are 36.0%, and accumulative total is used xylose mother liquid 2.54L.
With the fermentation liquid distillation, obtain alcohol, filtrate is collected in centrifugation then; Filter residue is made the DDGS feed through evaporation concentration, drying, granulation, packing.
Embodiment 2
Preparation xylose mother liquid 20% (m/v), yeast powder 0.5% (m/v), corn steep liquor 1.0% (m/v), potassium primary phosphate 0.05% (m/v), sal epsom 0.075% (m/v), tap water is settled to 1.08L, the 5L fermentor tank alcoholic fermentation medium of pH nature.
Sterilized 15 minutes for 110 ℃, insert the cultured gene engineering yeast liquid seeds of 0.12L (S.cerevisiae ZU-10) when being cooled to 30 ℃.Feed sterile air with 1: 0.6 velocity ratio, mixing speed 300rpm, cultivated about 11 hours for 30 ℃, cell concn optical density(OD) (O.D.) value is 58.8, stops ventilation, keeps mixing speed, culture temperature is increased to 33 ℃, add glucose concn that the mode of xylose mother liquid controls fermention medium in 1～2% (m/v) scope by stream, when the fermentation liquid volume reaches 3.5L, stop stream and add xylose mother liquid, continue to be cultured to fermentation ends.
Adopt gas Chromatographic Determination, ethanol concn reaches 5.27% (v/v) in the fermented liquid, and fermentation period 64 hours, sugar alcohol transformation efficiency are 39.9%, and accumulative total is used xylose mother liquid 2.54L.
With the fermentation liquid distillation, obtain alcohol, filtrate is collected in centrifugation then; Filter residue is made the DDGS feed through evaporation concentration, drying, granulation, packing.
Embodiment 3
Preparation xylose mother liquid 15% (m/v), yeast powder 0.5% (m/v), corn steep liquor 1.0% (m/v), potassium primary phosphate 0.05% (m/v), sal epsom 0.075% (m/v), tap water is settled to 0.96L, the 5L fermentor tank alcoholic fermentation medium of pH nature.
Sterilized 15 minutes for 110 ℃, inserting the cultured gene engineering yeast liquid seeds of 0.24L (S.cerevisiae ZU-10) when being cooled to 30 ℃ cultivates, elder generation feeds sterile air with 1: 0.6 velocity ratio, mixing speed 300rpm, cultivated about 9 hours for 30 ℃, cell concn optical density(OD) (O.D.) value is 52.9, stop ventilation, keep mixing speed, culture temperature is increased to 33 ℃, add glucose concn that the mode of xylose mother liquid controls fermention medium in 1～2% (m/v) scope by stream, when the fermentation liquid volume reaches 3.5L, stop stream and add xylose mother liquid, continue to be cultured to fermentation ends.
Adopt gas Chromatographic Determination, ethanol concn reaches 5.32% (v/v) in the fermented liquid, and fermentation period 64 hours, sugar alcohol transformation efficiency are 41.2%, and accumulative total is used xylose mother liquid 2.48L.
With the fermentation liquid distillation, obtain alcohol, filtrate is collected in centrifugation then; Filter residue is made the DDGS feed through evaporation concentration, drying, granulation, packing.
Embodiment 4
Preparation xylose mother liquid 7% (m/v), through centrifugal zymamsis distillation mash 21% (m/v), yeast powder 0.2% (m/v), peptone 0.1% (m/v), corn steep liquor 0.8% (m/v), potassium primary phosphate 0.1% (m/v), sal epsom 0.05% (m/v), tap water is settled to 3.15L, the 5L fermentor tank xylitol fermentation substratum of pH5.0.
Sterilized 10 minutes for 110 ℃, insert the cultured candiyeast liquid seeds of 0.35L when being cooled to 31 ℃.Feed sterile air with 1: 0.5 velocity ratio, mixing speed 300rpm, cultivated about 13 hours for 31 ℃, cell concn optical density(OD) (O.D.) value is 22.9, feed sterile air with 1: 0.3 velocity ratio, fermented 66 hours, finish fermentation, the Xylitol productive rate reaches 7.1%, and the sugar alcohol transformation efficiency reaches 72.1%.
Filtering fermentating liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again.
Embodiment 5
Preparation xylose mother liquid 7% (m/v), through centrifugal zymamsis distillation mash 37% (m/v), yeast powder 0.3% (m/v), peptone 0.1% (m/v), corn steep liquor 1.2% (m/v), potassium primary phosphate 0.1% (m/v), sal epsom 0.05% (m/v), tap water is settled to 3.15L, the 5L fermentor tank xylitol fermentation substratum of pH5.0.
Sterilized 10 minutes for 110 ℃, insert the cultured candiyeast liquid seeds of 0.35L when being cooled to 31 ℃.Feed sterile air with 1: 0.5 velocity ratio, mixing speed 300rpm, cultivated about 16 hours for 31 ℃, cell concn optical density(OD) (O.D.) value is 26.2, feed sterile air with 1: 0.3 velocity ratio, fermented 90 hours, finish fermentation, the Xylitol productive rate reaches 9.8%, and the sugar alcohol transformation efficiency reaches 65.5%.
Filtering fermentating liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again.
Embodiment 6
Preparation xylose mother liquid 8% (m/v), through centrifugal zymamsis distillation mash 21% (m/v), yeast powder 0.2% (m/v), peptone 0.1% (m/v), corn steep liquor 0.9% (m/v), potassium primary phosphate 0.1% (m/v), sal epsom 0.05% (m/v), tap water is settled to 3.15L, the 5L fermentor tank xylitol fermentation substratum of pH5.0.
Sterilized 10 minutes for 110 ℃, insert the cultured candiyeast liquid seeds of 0.35L when being cooled to 31 ℃.Feed sterile air with 1: 0.5 velocity ratio, mixing speed 300rpm, cultivated about 12 hours for 31 ℃, cell concn optical density(OD) (O.D.) value is 22.3, feed sterile air with 1: 0.3 velocity ratio, fermented 68 hours, finish fermentation, the Xylitol productive rate reaches 7.7%, and the sugar alcohol transformation efficiency reaches 74.8%.
Filtering fermentating liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again.
Embodiment 7
Preparation xylose mother liquid 8% (m/v), through centrifugal zymamsis distillation mash 35% (m/v), yeast powder 0.3% (m/v), peptone 0.1% (m/v), corn steep liquor 1.3% (m/v), potassium primary phosphate 0.1% (m/v), sal epsom 0.05% (m/v), tap water is settled to 3.15L, the 5L fermentor tank xylitol fermentation substratum of pH5.0.
Sterilized 10 minutes for 110 ℃, insert the cultured candiyeast liquid seeds of 0.35L when being cooled to 31 ℃.Feed sterile air with 1: 0.5 velocity ratio, mixing speed 300rpm, cultivated about 12 hours for 31 ℃, cell concn optical density(OD) (O.D.) value is 29.9, feed sterile air with 1: 0.3 velocity ratio, fermented 84 hours, finish fermentation, the Xylitol productive rate reaches 10.4%, and the sugar alcohol transformation efficiency reaches 70.4%.。
Filtering fermentating liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (9)
1. the treatment process of an xylose mother liquid is to utilize two-step fermentation, utilizes the glucose in the distillery yeast bacterial classification xylose-fermenting mother liquor to prepare alcohol earlier, distill alcohol; Utilize the wood sugar in the Xylitol barms fermentation mother liquor to prepare Xylitol then, fermented liquid successively extracts Xylitol and pectinose.
2. treatment process as claimed in claim 1 is characterized in that, may further comprise the steps:
1) with xylose mother liquid as carbon source, configuration glucose quality volumetric concentration is 2～3% alcoholic fermentation medium;
2) the distillery yeast bacterial classification is inoculated in the alcoholic fermentation medium cultivates, fermentating metabolism alcohol is reduced to the quality volumetric concentration below 0.3% until glucose concn;
3) fermentation liquid obtains alcohol through distillation, refilters to remove yeast and partial impurities;
4) filtrate and xylose mother liquid are mixed as carbon source, make that to contain the glucose quality volumetric concentration be 1.0～1.2%, and wood sugar quality volumetric concentration is 10～15% xylitol fermentation substratum;
5) the Xylitol barms is inoculated in the xylitol fermentation substratum cultivates, when residual wood sugar quality volumetric concentration is lower than 0.8% in the fermented liquid, finish fermentation; Fermentation ends after-filtration fermented liquid is removed yeast and partial impurities, and filtrate is used for successively extracting Xylitol and pectinose.
3. treatment process as claimed in claim 2 is characterized in that step 2) in, described cultivation is following to be carried out, and carries out aerobic earlier and cultivates, and feeds sterile air and stirring; Breed when yeast cell and stop logical sterile air when the OD value is 40～60, stream adds xylose mother liquid control glucose quality volumetric concentration 1～2% simultaneously; When the fermentation liquid volume reaches 60～90% liquid amounts, stop stream and add, continue fermentation and reduce to below 0.3% until the glucose quality volumetric concentration.
4. treatment process as claimed in claim 2 is characterized in that, in the step 5), described cultivation is following to be carried out, and carries out aerobic earlier and cultivates, and feeds sterile air and stirring; Breed when the OD value is 20～30 when yeast cell, change little oxygen over to and cultivate.
5. as claim 3 or 4 described treatment processs, it is characterized in that it is to feed sterile air and stirring in the culturing process that described aerobic is cultivated, the velocity ratio of described sterile air is 1: 0.4～1: 1.
6. treatment process as claimed in claim 4 is characterized in that, described micro-aerobe fermentation is to feed sterile air and stirring in the culturing process, and the velocity ratio of described sterile air is 1: 0.1～1: 0.3.
7. treatment process as claimed in claim 2 is characterized in that, in described alcoholic fermentation medium and the described xylitol fermentation substratum, also comprises nitrogenous source and inorganic salt, and used nitrogenous source is one or more in yeast powder, peptone, corn steep liquor, the urea; Used inorganic salt are one or more in sal epsom, the potassium primary phosphate.
8. treatment process as claimed in claim 2 is characterized in that, step 3) and 5) yeast and the partial impurities that obtain after filtering be used to prepare feed.
9. treatment process as claimed in claim 1 or 2 is characterized in that may further comprise the steps:
1) with xylose mother liquid as carbon source, configuration glucose quality volumetric concentration is 2～3% alcoholic fermentation medium;
2) the distillery yeast bacterial classification is inoculated into carries out aerobic in the spirituosity fermention medium and cultivate, feed sterile air and stirring, breed when yeast cell and to stop logical sterile air carry out zymamsis when the OD value is 40～60, stream adds xylose mother liquid control glucose quality volumetric concentration 1～2% simultaneously; When the fermentation liquid volume reaches 60～90% liquid amounts, stop stream and add, continue fermentation and reduce to below 0.3% until the glucose quality volumetric concentration;
3) fermentation liquid obtains alcohol through distillation, refilters to remove yeast and partial impurities;
4) filtrate and xylose mother liquid are mixed as carbon source, make that to contain the glucose quality volumetric concentration be 1.0～1.2%, and wood sugar quality volumetric concentration is 10～15% xylitol fermentation substratum;
5) the Xylitol barms is inoculated into aerobic yeast culture in the xylitol fermentation substratum, when yeast cell is bred the micro-aerobe fermentation stage that changes over to when the OD value is 20～30; When residual wood sugar quality volumetric concentration is lower than 0.8% in the fermented liquid, finish fermentation; Fermentation ends after-filtration fermented liquid is removed yeast and partial impurities, filtrate through decolouring, from hand over, concentrate, crystallization makes Xylitol, crystalline mother solution makes pectinose through simulation moving-bed, concentrated, crystallization again;
6) step 3) and step 5) are filtered the yeast and the partial impurities that obtain and be used as feed.
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| CN101921810A (en) * | 2010-06-11 | 2010-12-22 | 广西民族大学 | Method for preparing xylitol and L-arabinose mixed crystal from xylose mother liquid |
| CN102580611A (en) * | 2011-12-15 | 2012-07-18 | 重庆大学 | Method for processing xylose mother solutions |
| CN106591384A (en) * | 2016-12-21 | 2017-04-26 | 浙江华康药业股份有限公司 | Comprehensive treatment method of xylose mother liquor |
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| WO2024153506A1 (en) * | 2023-01-18 | 2024-07-25 | IFP Energies Nouvelles | Method for treating lignocellulosic biomass |
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