CN101775446A - Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar - Google Patents
Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar Download PDFInfo
- Publication number
- CN101775446A CN101775446A CN201010101585A CN201010101585A CN101775446A CN 101775446 A CN101775446 A CN 101775446A CN 201010101585 A CN201010101585 A CN 201010101585A CN 201010101585 A CN201010101585 A CN 201010101585A CN 101775446 A CN101775446 A CN 101775446A
- Authority
- CN
- China
- Prior art keywords
- sugar
- fermentalbe
- resin
- degradation
- glycosylated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to a technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar, which includes the procedures of drying and grinding of the white spirit waste lees, glycosylated degradation, the separation of saccharic acid, and the like. The technique is as follows: mixing ground waste lees with hydrogen chloride with mass fraction of 2% according to mass per unit volume of 1:10 for glycosylated degradation and collecting the filtrate; letting the filtrate pass through a chromatographic column which is filled with anionic resin, eluting through distilled water and collecting the eluate by step; and combining the eluates with sugar content equal to or more than 0.5 to be recovered sugar liquid. The recovered sugar liquid can be used as material for alcohol fermentation or other fermentations after being concentrated, and the used anionic exchange resin can be regenerated through NaOH. The concentration of the reducing sugar in the recovered sugar liquid prepared through the technique is equal to or more than 1%, wherein the content of dextrose is 55%, the content of xylose is 35% and the content of others is 10%; and the separation and recovery rate of the saccharic acid is more than 75%. The saccharic acid separation process is low in cost and no harmful impurities such as sulfate radical and the like are left behind, so the fermentalbe sugar has little effect to the subsequent alcohol fermentation or other fermentations. Therefore, the fermentalbe sugar is ideal material for alcohol fermentation and other fermentations.
Description
Technical field
The present invention relates to a kind of glycosylated degradation of white spirit and lose poor technology, particularly a kind of novel process of efficiently saccharifying degradation of white spirit waste lees to prepare fermentalbe sugar belongs to the light industry biological technical field.
Background technology
China is a drinks production and consumption big country.The scale operation of liquor, when satisfying market demand and accumulating a large amount of construction funds for development and national economy, the fermentation that has produced enormous amount is lost poor.Contain a large amount of organism owing to lose in poor,, vinasse are abandoned as refuse, both wasted resource, cause serious environmental to pollute pressure again as starch, Mierocrystalline cellulose and organic acid etc.The main mode of utilizing of present domestic spirit distiller grain comprises: be used for former wine and produce, produce glycerine, cultivation edible mushrooms again, extract preparation phytic acid isoreactivity material, fermentation recovery biogas, production feedstuff protein or the like.Yet in these processing modes, except being used as feed, agricultural fertilizer, additive method mostly is difficult to fundamentally solve the final whereabouts problem of vinasse, and might produce more poor slag.Lose poor complicated component in addition, the water content height, difficult storage has the fermentation weighting materials such as rice husk that are difficult for utilization again, so still there is certain difficulty in the utilization of spirit distiller grain.
Meanwhile, along with the minimizing gradually of Nonrenewable resources such as world oil and the increase day by day of energy demand pressure, seek reproducible substitute energy such as alcohol fuel, biofuel etc. and receive increasing concern.Spirit distiller grain is carried out the efficiently saccharifying degraded, be not only the effective way of liquor production offal treatment, but also the carbon source of high-quality cheapness can be provided for the fermentative production of fuel alcohol equal energy source.
Song Andong etc. have reported experimental study [the Transactions of the Chinese Society of Agricultural Engineering .2003 that utilizes the vinasse biomass ferment to produce alcohol fuel, 19 (4): 278-281], its main contents are carried out ethanol fermentation for adopting prozyme directly to transform spirit distiller grain, but its result of study shows, directly utilize the starch and the cellulosic interest rate of spirit distiller grain fermentative production of ethanol to be respectively 2% and 4%, its utilization ratio is all lower.Secondly, Mo Kai etc. to the part technology of the glycosylated degradation of spirit distiller grain carried out preliminary discussion [preparation condition of spirit distiller grain glycosylated degradation liquid is inquired into. brewing science and technology .2007,160 (10): 85-87.], but do not form spirit distiller grain from pre-treatment, glycosylated degradation to the isolating complete process of saccharic acid.Therefore, propose a kind of efficiently saccharifying degradation of white spirit and lose poor technology, be used for zymamsis or as the raw materials for production of other fermentations, task of the present invention just place with the preparation fermentable sugars.
Summary of the invention
Purpose of the present invention has existing deficiency in the spirit distiller grain technology now in order to overcome just, and provides a kind of efficiently saccharifying degradation of white spirit to lose the poor technology that obtains fermentable sugars.This technology not only sugar yield and the sugared rate of recovery is higher, and the saccharic acid separation costs is lower, and detrimental impurity such as sulfate radical-free is residual, and is less to follow-up alcohol or the influence of other fermentation manufacturing techniques.
For realizing the purpose of foregoing invention, the technical scheme that the present invention's employing is made of following technical measures realizes.
The technology of a kind of glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar of the present invention comprises following processing step:
(1) lose poor drying:
With water content is 60～70% fresh spirit distiller grain, and oven dry to its water content is not more than 10% under 90～100 ℃ of temperature, places dry shady and cool place to preserve standby;
(2) lose poor fine pulverizing:
Above-mentioned spirit distiller grain is after drying carried out fine pulverizing, require it can pass through 40 order sub-sieves more than 90%;
(3) dilute hydrochloric acid glycosylated degradation:
With the above-mentioned spirit distiller grain fine powder of selecting through sub-sieve and the hydrogenchloride of massfraction 2%, according to 1: 10 mixed of mass volume ratio, glycosylated degradation is 45～60 minutes under 120 ℃ of temperature, and suction filtration is removed solid residue wherein then, and collects filtrate;
(4) saccharic acid separates:
The filtrate that above-mentioned collection is obtained is by filling the chromatography column of resin anion(R.A), and carry out wash-out by the speed of per minute 1.2%～1.5% resin volume with distilled water, the fraction collection elutriant, simultaneously with the pol in the saccharometer measurement elutriant, in elutriant, detect less than till the pol, the elutriant that merges pol 〉=0.5 has promptly made and can be used for zymamsis or as the fermentable sugars of other fermentations;
(5) regeneration of anionite-exchange resin:
The hydrochloric acid that residues in the chromatography column is neutral with flushing with clean water to its pH, soaked resin 4～6 hours with the sodium hydroxide solution that is the 5g/100ml of 2～3 times of volumes of resin again, be neutral with the abundant drip washing of distilled water until water outlet pH then, this anionite-exchange resin can be used for saccharic acid once more and separate.
In the technique scheme, the weighting material of the chromatography column of described filling resin anion(R.A) is the macropore weak basic anion exchange resin, and its loading level is 1.5～2 times of above-mentioned (3) filtrate volume collected of step.
In the technique scheme, the diameter of the chromatography column of described filling resin anion(R.A) and its interior height ratio of filling anionite-exchange resin are 1: 6～10.
Sugar of the present invention is reclaimed liquid concentrate, and after regulating pH, promptly can be used as the carbon source material of zymamsis or other fermentative production.
The present invention has following characteristics and beneficial technical effects:
1, the glycosylated degradation of white spirit that adopts of the present invention is lost poor technology and can be obtained higher sugar yield, and reducing sugar is higher than 20% for the yield of spirit distiller grain sample dry weight, and the reducing sugar rate of recovery of anion exchange separation saccharic acid can reach more than 75%.
2, the dilute hydrochloric acid degraded adopted of the present invention and macropore weak base anion exchange column carry out saccharic acid and separate, and its separation costs is lower, and detrimental impurity such as sulfate radical-free is residual, and be less to follow-up zymamsis or the influence of other fermentative production.
3, the technology gained sugar of the present invention's employing reclaims concentration of reduced sugar 〉=1% in the liquid, and wherein glucose 55%, wood sugar 35%, and other are 10% years old.
4, the present invention utilizes anionite-exchange resin to separate saccharic acid, and not only rate of recovery height, and anionite-exchange resin is reusable, thereby can reduce production costs.
Description of drawings
Fig. 1 secondary of the present invention is lost the pol change curve of poor glycosylated degradation liquid elution process;
Fig. 2 the present invention once loses the pol change curve of poor glycosylated degradation liquid elution process.
Embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the content of the invention described above.
The used spirit distiller grain of this example is lost poor for the secondary that China five-Grain Liquor brewery provides; Used anionite-exchange resin model is a D301 macropore weak basic anion exchange resin.
(1) lose poor drying:
With fresh water content 65.5%, thick starch 16.91%, robust fibre 22%, the secondary liquor fermentation of ash 15.62% is lost poor 100g, and in 90 ℃ of temperature oven dry, its water content is 6% after measured, broken the making of waste spent grains powder lost poor fine powder, place dry shady and cool place to preserve standby;
(2) lose poor fine pulverizing:
Cross 40 order sub-sieves with above-mentioned through the waste spent grains powder 30g after the drying and crushing, its ratio of sieving is 92.65%;
(3) dilute hydrochloric acid glycosylated degradation:
2% hydrogenchloride (HCl) that takes by weighing above-mentioned spirit distiller grain powder 25g and massfraction and be is that 1: 10 mixed gets mixture according to mass volume ratio, and glycosylated degradation is 45 minutes under 120 ℃ of temperature; Suction filtration is removed solid residue, collects filtrate, and concentration of reduced sugar is 2.82% in the mensuration hydrolyzed solution, and glucose concn is 1.66%, and xylose concentration is 0.96%;
(4) saccharic acid separates:
The mixture suction filtration that dilute hydrochloric acid degraded back produces is removed solid residue, collects and obtain filtrate 189.5ml, with this filtrate by being filled with the chromatography column of 322.4ml D301 macropore weak basic anion exchange resin, the high 30cm of its packed column, diameter 3.7cm; And carry out wash-out with the speed of 4ml/min with distilled water, and with 40ml unit fraction collection elutriant, measure pol in the elutriant with saccharometer simultaneously, till detecting less than sugar.The elutriant of pol 〉=0.5 is merged, obtain 402ml sugar altogether and reclaim liquid, the concentration of reduced sugar of measuring wherein is 1.05%, and glucose concn is 0.59%, and xylose concentration is 0.36%.As calculated, in reducing sugar, the isolating sugared rate of recovery of saccharic acid is 78.99%, and its pH value is 9; Figure 1 shows that the variation of pol in the embodiment elutriant, as can be seen from Figure, its pol can obviously be measured in the collection tube of 170～600mL;
(5) regeneration of anionite-exchange resin: the hydrochloric acid that will residue in the chromatography column post is extremely neutral with flushing with clean water, sodium hydroxide solution with 800ml 5g/100ml soaked resin 5 hours then, be neutral with the abundant drip washing of distilled water until water outlet pH value then, this anionite-exchange resin can be used for saccharic acid once more and separate;
It is more than 5% that sugar recovery liquid of the present invention is concentrated into glucose concn, and regulates pH value to 3.0～4.0, inserts liquor-making yeast, promptly can be used for zymamsis.
The spirit distiller grain that the used spirit distiller grain of this example provides for China Quanxing brewery; Used anionite-exchange resin model is a D301 macropore weak basic anion exchange resin.
(1) lose poor drying:
With water content 65%, thick starch 18.05%, robust fibre 35.43%, a spirit distiller grain 100g of ash 13.48% is dried to water content approximately 5% under 90 ℃ of temperature, its pulverizing is made lose poor fine powder, places dry shady and cool place to preserve standby;
(2) lose poor fine pulverizing;
To cross 40 order sub-sieves through the waste spent grains powder 30g after the drying and crushing, the ratio of sieving is 94.52%;
(3) dilute hydrochloric acid glycosylated degradation:
Take by weighing above-mentioned waste spent grains powder 10g and massfraction and be 2% hydrogenchloride (HCl), get mixture according to 1: 10 mixed of mass volume ratio, glycosylated degradation is 60 minutes under 120 ℃ of temperature, suction filtration is removed solid residue, collect filtrate, concentration of reduced sugar is 2.26% in the mensuration hydrolyzed solution, and glucose concn is 1.33%, and xylose concentration is 0.83%;
(4) saccharic acid separates:
The mixture suction filtration that dilute hydrochloric acid degraded back produces is removed solid residue, collection obtains filtrate 79.6ml, with chromatography column (the packed column high 30cm of this filtrate by being filled with 322.4ml D301 macropore weak basic anion exchange resin, diameter 3.7cm,) and carry out wash-out with distilled water with the 4ml/min flow velocity, with 20ml is unit fraction collection elutriant, simultaneously with the pol in the saccharometer measurement elutriant, till detecting less than sugar; The elutriant of pol 〉=0.5 is merged, obtain 146ml sugar altogether and reclaim liquid, the concentration of reduced sugar of measuring wherein is 1.002%, and glucose concn is 0.55%, and xylose concentration is 0.39%, as calculated, in reducing sugar, the isolating sugared rate of recovery of saccharic acid is 81.4%, and the pH value then is elevated to about 9 by 0.5 simultaneously, Figure 2 shows that the pol in this example elution process changes, and can obviously measure in the collection tube of its reducing sugar between 167～345mL as can be seen from Figure.
(5) regeneration of anionite-exchange resin:
The hydrochloric acid that residues in the chromatography column post is extremely neutral with flushing with clean water, sodium hydroxide solution with 800ml 5g/100ml soaked resin 5 hours, be neutral with the abundant drip washing of distilled water until water outlet pH value then, this anionite-exchange resin can be used for saccharic acid once more and separate;
It is more than 5% that sugar recovery liquid of the present invention is concentrated into glucose concn, and regulates pH value to 3.0～4.0, inserts liquor-making yeast, promptly can be used for zymamsis.
Claims (3)
1. the technology of a glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar is characterized in that comprising following processing step:
(1) lose poor drying:
With water content is 60～70% fresh spirit distiller grain, and oven dry to its water content is not more than 10% under 90～100 ℃ of temperature, places dry shady and cool place to preserve standby;
(2) lose poor fine pulverizing:
Above-mentioned spirit distiller grain is after drying carried out fine pulverizing, require it can pass through 40 order sub-sieves more than 90%;
(3) dilute hydrochloric acid glycosylated degradation:
With the above-mentioned spirit distiller grain fine powder of selecting through sub-sieve and the hydrogenchloride of massfraction 2%, according to 1: 10 mixed of mass volume ratio, glycosylated degradation is 45～60 minutes under 120 ℃ of temperature, and suction filtration is removed solid residue wherein then, and collects filtrate;
(4) saccharic acid separates:
The filtrate that above-mentioned collection is obtained is by filling the chromatography column of resin anion(R.A), and carry out wash-out by the speed of per minute 1.2%～1.5% resin volume with distilled water, the fraction collection elutriant, simultaneously with the pol in the saccharometer measurement elutriant, in elutriant, detect less than till the pol, the elutriant that merges pol 〉=0.5 has promptly made and can be used for zymamsis or as the fermentable sugars of other fermentations;
(5) regeneration of anionite-exchange resin:
The hydrochloric acid that residues in the chromatography column is neutral with flushing with clean water to its pH, soaked resin 4～6 hours with the sodium hydroxide solution that is the 5g/100ml of 2～3 times of volumes of resin again, be neutral with the abundant drip washing of distilled water until water outlet pH then, this anionite-exchange resin can be used for saccharic acid once more and separate.
2. the technology of glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar according to claim 1, the weighting material that it is characterized in that the chromatography column of described filling resin anion(R.A) is the macropore weak basic anion exchange resin, and its loading level is 1.5～2 times of the filtrate volume collected;
3. the technology of glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar according to claim 1 is characterized in that diameter and its interior height ratio of filling anionite-exchange resin of the chromatography column of described filling resin anion(R.A) is 1: 6～10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010101585A CN101775446A (en) | 2010-01-27 | 2010-01-27 | Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010101585A CN101775446A (en) | 2010-01-27 | 2010-01-27 | Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101775446A true CN101775446A (en) | 2010-07-14 |
Family
ID=42512032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010101585A Pending CN101775446A (en) | 2010-01-27 | 2010-01-27 | Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101775446A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088166A (en) * | 2013-01-28 | 2013-05-08 | 山东省食品发酵工业研究设计院 | Method for extracting xylose by strong-flavor solid white wine vinasse |
| CN103103219A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains acid hydrolysis liquid glucose and preparation process thereof |
| CN103103218A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains alkaline hydrolysis liquid glucose and preparation process thereof |
| CN103100370A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains acid-base modified adsorption material and preparation process thereof |
| CN109234199A (en) * | 2018-10-22 | 2019-01-18 | 四川大学 | A kind of caproic acid bacterium culture medium containing liquor fermentation process raw material and its application |
-
2010
- 2010-01-27 CN CN201010101585A patent/CN101775446A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103219A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains acid hydrolysis liquid glucose and preparation process thereof |
| CN103103218A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains alkaline hydrolysis liquid glucose and preparation process thereof |
| CN103100370A (en) * | 2011-11-10 | 2013-05-15 | 西南科技大学 | Distillers' grains acid-base modified adsorption material and preparation process thereof |
| CN103100370B (en) * | 2011-11-10 | 2015-01-28 | 西南科技大学 | Distillers' grains acid-base modified adsorption material and preparation process thereof |
| CN103103218B (en) * | 2011-11-10 | 2015-07-08 | 西南科技大学 | Distillers' grains alkaline hydrolysis liquid glucose and preparation process thereof |
| CN103103219B (en) * | 2011-11-10 | 2015-07-08 | 西南科技大学 | Distillers' grains acid hydrolysis liquid glucose and preparation process thereof |
| CN103088166A (en) * | 2013-01-28 | 2013-05-08 | 山东省食品发酵工业研究设计院 | Method for extracting xylose by strong-flavor solid white wine vinasse |
| CN103088166B (en) * | 2013-01-28 | 2014-04-30 | 山东省食品发酵工业研究设计院 | Method for extracting xylose by strong-flavor solid white wine vinasse |
| CN109234199A (en) * | 2018-10-22 | 2019-01-18 | 四川大学 | A kind of caproic acid bacterium culture medium containing liquor fermentation process raw material and its application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102352381B (en) | Method using xylose production waste liquid to produce acetone and butanol | |
| CN102251010B (en) | Method for producing ethanol by high-efficiency simultaneous saccharification and cofermentation | |
| CN101497904B (en) | Method for producing xylitol and arabinose at the same time | |
| CN101974570B (en) | Method for recycling cellulose complete components in fuel ethanol production | |
| CN101775446A (en) | Technique for glycosylated degradation of white spirit waste lees to prepare fermentalbe sugar | |
| CN103100260B (en) | Efficient method for separating solid residue and product in lignocellulose fermented mash | |
| MXPA05010825A (en) | Process for producing sugar and useful substance. | |
| CN104109694A (en) | Method for comprehensively utilizing sweet sorghum straws | |
| CN103773812B (en) | A kind of Fructus Querci acutissimae prepares the method for alcohol fuel and recycling | |
| CN101165189A (en) | Meso one-step method ethanol production method for potato raw starch | |
| CN106399393B (en) | Method for producing fuel ethanol based on irradiation pretreatment of straws | |
| CN101235390B (en) | Method for producing fuel ethanol by solid fermentation of sugar grass straw | |
| CN102154390B (en) | Method for producing ethyl acetate by taking starchiness as main raw materials | |
| CN110564780B (en) | Method for co-production of biogas by fermenting ethanol with bagasse-molasses-yam residue mixed raw material | |
| CN105400830A (en) | Method for producing ethyl alcohol through lignocellulose raw material | |
| CN112522328A (en) | Method for preparing ethanol by using degradable waste | |
| CN101358213B (en) | Method for producing energy ethanol by fermentation of waste paper pulp | |
| CN102296092B (en) | Pretreatment method for sugarcane juice alcoholic fermentation broth and extraction method for high value products in waste liquid | |
| CN102181510B (en) | Technological process for producing ethanol through steam explosion and fermentation of trunks and branches of poplar trees | |
| CN102476128B (en) | Method for green conversion of urban and rural household reuse into renewable energy sources | |
| CN101870715B (en) | Ether energy and preparation method and application thereof | |
| CN103074407A (en) | Novel method for increasing yield of fuel ethanol produced by straw | |
| CN109706273A (en) | A kind of method of phosphorus pentoxide catalysis lignocellulosic hydrolysed ferment | |
| CN115611711B (en) | Comprehensive utilization method of magnolia bark dregs | |
| CN101914590A (en) | Detoxification and fermentation method by co-use of West issatchenkia terricola and Candida tropicalis and production preparation process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20100714 |