CN1319980C - Process for preparing crystalline xylose by hydrolysis of maize peel - Google Patents
Process for preparing crystalline xylose by hydrolysis of maize peel Download PDFInfo
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- CN1319980C CN1319980C CNB2005100827829A CN200510082782A CN1319980C CN 1319980 C CN1319980 C CN 1319980C CN B2005100827829 A CNB2005100827829 A CN B2005100827829A CN 200510082782 A CN200510082782 A CN 200510082782A CN 1319980 C CN1319980 C CN 1319980C
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Abstract
The present invention relates to a method for preparing crystalline xylose by hydrolyzing maize peels, which comprises the following steps: preprocessing maize peels by 0.5 to 1 mL/kg of amylase with high temperature resistance to dissolve out starch contained in the maize peels so as to obtain liquefied dregs of maize peels; boiling the liquefied dregs of the maize peels by 1.2 to 2.0% of H2 SO4 at normal pressure for hydrolyzation, wherein the hydrolyzate contains 55 to 75% of total reducing sugar; crystallizing the hydrolyzate, and adding xylose crystal seeds during crystallization, wherein the amount of added crystal seeds is 20 to 40% of the total xylose amount of the massecuite. In the present invention, maize peels are used as raw materials to produce crystalline xylose, which solves the problem that when used as raw materials to produce crystalline xylose, corn cobs need piling at large areas and have severe pollution. The raw materials of maize peels are preprocessed by little amount of amylase with high temperature resistance, so that starch contained in the maize peels is dissolved out, and little dextrose is produced during the hydrolyzation of the maize peels. The maize peels without starch are boiled at normal pressure for hydrolyzation, which avoids the method of hydrolyzing corn cobs at 125 to 130 DEG C, prevents xylose damage and side reaction, and greatly reduces the purification cost of xylose solution.
Description
Technical field
The present invention relates to a kind of method of preparing crystalline xylose by hydrolysis of maize peel.
Background technology
Along with expanding economy and the people concern to health, functional sugar-free sweet food product have become the foodstuffs industry new growth point.As the sugar alcohol (comprising Xylitol, sorbyl alcohol, maltose alcohol etc.) of sugar substitute, admitted by the human consumer gradually.Wherein Xylitol is the unique kind of function, and international grain farmer and health organization CAC approval Xylitol etc. are the sugar substitute of not limited amount.China produces Xylitol country early, since the seventies outlet in last century, is Xylitol production and big export country in decades always.Xylitol is to be raw material in order to contain the high corn cob of hemicellulose, extracts wood sugar earlier, then the wood sugar hydrogenation is generated Xylitol, so along with the development of Xylitol, as the crystalline xylose of Xylitol raw material, also obtain corresponding development.China's crystalline xylose from 1970 less than tens tons, produce per year to crystalline xylose in 2004 and to reach 30,000 tons, except that as the Xylitol raw material, partly also be used for non-caloric sweetener and export to foreign countries.Approximately per 10 tons of corn cobs can be made 1 ton of crystalline xylose.Enterprise needs the big content of starting materials of purchase for guaranteeing stably manufactured.Smallest size is produced 1000 tons wood sugar enterprise, 10,000 tons of corn cobs of also minimum purchase in every year per year.Will there be enough places, the storage of raw materials in enterprise.Year in year out, up to ten thousand tons of corn cobs are deposited in the open, blowing and raining, and the loss of not only going mouldy, and corn cob adhered to a large amount of dust has brought the heavy peace and quiet load of raw material corn cob to production, has increased water consumption and blowdown flow rate.Recently because corn cob is emulatively rushed to purchase in another exported product furfural volume increase.Because corn cob can replace rural area fuel, make the procurement price of corn cob sharp rise simultaneously.Seek new, stable, clean, cheap raw material sources, be the urgent problem that the Xylitol industry is often discussed in recent years for this reason.
Maize peel claims zein fiber again, is the crust of corn grain, is the by product of corn processed starch factory, accounts for about 10% of corn gross weight.China's W-Gum industry year processing corn is 1,000 ten thousand tons at present, and maize peel estimates at more than 100 ten thousand tons, is dispersed in the W-Gum factory of each provinces and regions, the whole nation.The W-Gum source mill that some is large-scale produces maize peel per year and can reach more than 30,000 tons, thus maize peel as the wood sugar raw material, principle stable, clean with meeting fully, cheap raw material.
Though but maize peel is much cleaner than corn cob, in the contained reducing sugar, the wood sugar proportion is also than the much less in the corn cob after the maize peel hydrolysis.In the reducing sugar after the corn cob hydrolysis, wood sugar accounts for more than 75% (weight percent), is easy to crystallize out, and after the maize peel hydrolysis in the contained reducing sugar, and wood sugar is less than half, and particularly maize peel is residual a large amount of starch, and this brings difficulty to its deep processing and utilization.According to U.S.'s report, maize peel constitutes: Mierocrystalline cellulose 11%, hemicellulose 35%, glucose 32% (wherein 23% is that residual starch produces), protein 11.3%, lipid 6%, ash content 1.2%.W-Gum factory all handles maize peel as roughage both at home and abroad for a long time, is worth not high.
Many starch are arranged owing to maize peel is residual, and contain higher hemicellulose, so after the maize peel hydrolysis, its total reducing sugars productive rate is higher, and the test report was once used 2% sulphuric acid hydrolysis maize peel all more than 60% in 1984 as environmental protection institute of former China National Light Industrial Products Department both at home and abroad, its total reduzate productive rate is 65%, but its total reduzate is a kind of mixture of many kinds sugar, and wherein wood sugar is difficult to extract less than half.
According to nearest high pressure liquid chromatographic analysis, the mixing reducing sugar after the maize peel hydrolysis, wherein constituting of three kinds of main sugar: glucose 33.3%, wood sugar 42.7%, pectinose 22.8%.This mixing sugar, glucose accounts for 1/3, separate wherein some sugar separately, all acquires a certain degree of difficulty, thereby its utility value is greatly reduced.Commonplace generally acknowledged mixing sugar is utilized approach, it is the system fodder yeast, because have only fodder yeast could utilize multiple sugar to do nutrition, general per 2 tons of mixing sugar, can obtain 1 ton of fodder yeast, it is not high to rise in value, and has a lot of maize peel hydrolysis system fodder yeast researchs to report though the native land is inside and outside, does not see production.
In the mixing sugar after above-mentioned maize peel hydrolysis, containing the wood sugar about 30-40%, should be that added value is arranged most, and the sugar products kind of certain market capacity is arranged.Is problem that the glucose that how will influence xylose crystalline separates in advance? how to reduce the generation of the pollutent of liquid glucose effectively? and the ratio that how wood sugar is taken advantage at crystallisation process? only overcome the above problems, could make maize peel produce crystalline xylose cost-effectively becomes possibility.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, providing a kind of is the method for raw material production crystalline xylose with the maize peel.
Technical solution of the present invention is: a kind of method of preparing crystalline xylose by hydrolysis of maize peel is a raw material with the maize peel, may further comprise the steps:
(1) maize peel is used the pre-treatment of 0.5-1mL/kg fire resistant alpha-diastase, made starch stripping contained in the maize peel, obtain maize peel liquefaction slag;
(2) maize peel is liquefied slag 1.2-2.0%H
2SO
4Atmospheric boiling hydrolysis, hydrolysate comprise total reducing sugars 55-75%;
(3) with the hydrolysate crystallization, add the wood sugar crystal seed during crystallization, adding crystal seed amount is the 25-40% to total reducing sugar amount in the massecuite.
Usefulness of the present invention is:
1, is the raw material production crystalline xylose with the maize peel, overcome with the corn cob and stacked raw material and the serious problem of contamination of raw material for the raw material production crystalline xylose needs large stretch of place;
2, the raw material maize peel makes the stripping of maize peel starch contained therein, the generating capacity of the glucose when having reduced the maize peel hydrolysis with the pre-treatment of minute quantity fire resistant alpha-diastase;
3, removed the later maize peel of starch, used the atmospheric boiling hydrolysis, 125-130 ℃ of hydrolysis having avoided present corn cob to adopt prevented that wood sugar from destroying and side reaction produces, and reduces the purification cost of liquid glucose significantly.
Describe the present invention in detail below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
1, maize peel liquefaction: solid-to-liquid ratio 1: 8-12, add the high temperature resistant liquefaction enzyme of 0.5-1mL/kg, in high temperature 103-110 ℃, keep the 5-15 branch, then in 85-90 ℃ of insulation 1-2.5 hour.Liquefaction leachable 15-30%, wherein glucose 15-20% remains liquefaction slag 70-85%; The slag that will liquefy squeezing washing;
2, the liquefaction pulp water is separated: use concentration 1.2-2.0%H
2SO
4, solid-to-liquid ratio 1: 8-12, atmospheric boiling 3-4 hour, hydrolysis stripping total reducing sugars 55-70%, wherein wood sugar 30-45%;
3, neutralization: 70-80 ℃ of reaction 30-50 minute, be neutralized to PH3-3.3 with lime carbonate, mineral acid is below 0.1%.Filter;
4, decolouring: at 70-80 ℃, use activated carbon decolorizing, to transparence 85-95% to reducing sugar 3-5%.
5, ion exchange resin purifies: deviate from protein and mineral substance, and Yang-Yang-negative resin combination, load 0.5-1kg/kg is to transparence 95-100%;
6, prevapourising: outer heating evaporation under the vacuum makes reduzate be concentrated into 40-50%;
7, secondary decolourization: use activated carbon decolorizing, to transparence 95-100% to reducing sugar 1-2%;
8, final concentrating: be concentrated into 70-85% under the vacuum fast and obtain massecuite, prepare crystallization;
9, crystallization: press massecuite concentration and wood sugar content and add the wood sugar crystal seed, the add-on of wood sugar crystal seed is the 20-40% of crystal seed to total reducing sugar amount in the massecuite.With the per hour cooling of the speed below 1 ℃, reduce to 20-30 ℃, centrifugation acquisition crystalline xylose from 60-65 ℃.
Embodiment:
One, maize peel liquefaction
Feed intake: maize peel dry amount 2000g, solid-to-liquid ratio 1: 10 adds the high temperature resistant liquefaction enzyme liquefaction of 0.6mL/kg, makes the abundant stripping of starch.
1,90 ℃ of soaking times are 1 hour, the dry total amount that liquefies out 333g, the liquefaction dry rate of recovery 16.6%, the liquefaction slag rate of recovery 83.4%;
2,90 ℃ of soaking times are 1.8 hours, the dry total amount that liquefies out 472g, the liquefaction dry rate of recovery 23.6%, the liquefaction slag rate of recovery 76.4%.
Two, maize peel liquefaction pulp water is separated
1, drop into liquefaction slag dry amount 1429g, hydrolysising condition: sulfuric acid concentration 1.5%, atmospheric boiling were held time 3.5 hours, get hydrolyzed solution volume 15200ml, hydrolyzed solution dry concentration 6.8%, total acid 1.75%, reducing sugar (mixing sugar) 57.32%, reducing sugar dry weight 592.2g.Hydrolytic residue dry weight 708g;
2, drop into liquefied residue dry amount 1579g, hydrolysising condition: sulfuric acid concentration 1.5%, atmospheric boiling were held time 4 hours, get hydrolyzed solution volume 13500ml, hydrolyzed solution dry concentration 9.0%, total acid 2.0%, reducing sugar (mixing sugar) 63%, reducing sugar dry weight 765.45g.Hydrolytic residue dry weight 602g.
Three, purify: by above-mentioned processing requirement, hydrolyzed solution neutralizes through lime carbonate, activated carbon decolorizing, and ion exchange resin purifies, and evaporation concentration is to concentration 72-78%.
Four, crystallization:
1, concentration 72.5% massecuite 1200ml contains total reducing sugars 870ml, proportion 1.38, and reducing sugar is 1200g, contains wood sugar 49% in the total reducing sugars, wood sugar is 588g; Add wood sugar crystal seed 450g, be massecuite 37.5%, total reducing sugars is brought up to 1200g+450=1650g, and the wood sugar total amount is 588g+450=1038, and wood sugar accounts for total reducing sugars and brings up to 62.9% from 49%;
Be cooled to 30 ℃ from 60 ℃, totally 35 hours, drop into whizzer and separate, the 649g crystallization, remove crystal seed receive crystalline xylose 225.6g.
The crystalline xylose rate of recovery is 18.75% to the massecuite reducing sugar.
2, concentration 73.8%, and massecuite 1200ml, reducing sugar are 885ml, and proportion 1.385, reducing sugar heavily are 1221g,
Contain wood sugar 49.26%, wood sugar is 600g;
Add wood sugar crystal seed 500g, be massecuite 41.6%, total reducing sugars is brought up to 1221g+500=1721g wood sugar total amount 600+500=1100g, and wood sugar accounts for total reducing sugars and brings up to 63.9% from 49.26%,
Be cooled to 25 ℃ from 62 ℃, totally 40 hours, drop into whizzer and separate, the 715g crystalline xylose, remove crystal seed receive crystalline xylose 215g, the crystalline xylose rate of recovery is 17.6% to the massecuite reducing sugar.
3, concentration 81%, and massecuite 1657g, reducing sugar are 1342g heavily, contain wood sugar 48.5%, and wood sugar is 650.87g;
Add wood sugar crystal seed 300g, be massecuite 22.3%, total reducing sugars is brought up to 1342g+300=1642g wood sugar total amount 650.87+300=950.87g, wood sugar accounts for total reducing sugars and brings up to 55.3% from 48.5%, is cooled to 22 ℃, totally 41 hours from 63 ℃, the input whizzer separates, the 585g crystalline xylose, remove crystal seed receive crystalline xylose 285g, the crystalline xylose rate of recovery is 21.2% to the massecuite reducing sugar.
Claims (7)
1, a kind of method of preparing crystalline xylose by hydrolysis of maize peel is characterized in that with the maize peel being raw material, may further comprise the steps:
(1) maize peel is used the pre-treatment of 0.5-1mL/kg fire resistant alpha-diastase, made starch stripping contained in the maize peel, obtain maize peel liquefaction slag;
(2) maize peel is liquefied slag 1.2-2.0%H
2SO
4Atmospheric boiling hydrolysis, hydrolysate comprise total reducing sugars 55-75%;
(3) with the hydrolysate crystallization, add the wood sugar crystal seed during crystallization, adding crystal seed amount is the 25-40% to total reducing sugar amount in the massecuite.
2, method according to claim 1 is characterized in that also comprising (2) one-step hydrolysis product is neutralized with lime carbonate.
3, method according to claim 1 is characterized in that also comprising to (2) one-step hydrolysis product activated carbon decolorizing.
4, method according to claim 1 is characterized in that also comprising that (2) one-step hydrolysis product is carried out ion exchange resin to be purified.
5, method according to claim 1 is characterized in that concentrating earlier before the crystallization.
6, method according to claim 5 is characterized in that concentrating and carries out in two steps, and the first step makes reduzate be concentrated into 40-50%, and second step made reduzate be concentrated into 70-85%.
7, method according to claim 6 is characterized in that carrying out activated carbon decolorizing after the first step concentrates.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100827829A CN1319980C (en) | 2005-07-12 | 2005-07-12 | Process for preparing crystalline xylose by hydrolysis of maize peel |
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| CNB2005100827829A CN1319980C (en) | 2005-07-12 | 2005-07-12 | Process for preparing crystalline xylose by hydrolysis of maize peel |
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| CN1699389A CN1699389A (en) | 2005-11-23 |
| CN1319980C true CN1319980C (en) | 2007-06-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102116A (en) * | 2010-12-21 | 2011-06-22 | 山东省鲁洲食品集团有限公司 | Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391065B (en) * | 2011-08-09 | 2014-02-05 | 山东省鲁洲食品集团有限公司 | Method for producing dihydric alcohol and low molecular polyalcohol by taking corn husk as raw material |
| CN102351915B (en) * | 2011-08-11 | 2014-12-24 | 甘肃赫原生物制品有限公司 | Method for extracting xylose from xylose molasses |
| CN102534053B (en) * | 2011-12-23 | 2013-07-03 | 甘肃赫原生物制品有限公司 | Method for improving xylose crystallization yield |
| CN102524647B (en) * | 2012-03-13 | 2013-05-22 | 山东福田科技集团有限公司 | Calorie-free sweetener and preparation method thereof |
| CN103750139B (en) * | 2013-12-31 | 2015-08-19 | 吉林中粮生化有限公司 | A kind of straightforward procedure removing starch in wet milling of corn fiber |
Citations (1)
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| CN1446784A (en) * | 2003-04-10 | 2003-10-08 | 长春工业大学 | Method for producing xylitol by using bracteal leaf of maize |
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2005
- 2005-07-12 CN CNB2005100827829A patent/CN1319980C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1446784A (en) * | 2003-04-10 | 2003-10-08 | 长春工业大学 | Method for producing xylitol by using bracteal leaf of maize |
Non-Patent Citations (6)
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| 玉米深加工及综合利用 胡广民等，现代化农业，第10期 1996 * |
| 玉米皮半纤维素提取工艺的研究 王遂等，中国粮油学报，第15卷第3期 2000 * |
| 玉米芯制木糖醇生产工艺的优化研究 李琰等，郑州工程学院学报，第25卷第1期 2004 * |
| 用玉米芯制取木糖醇的工艺研究 荆文尧等，农机化研究，第4期 1995 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102116A (en) * | 2010-12-21 | 2011-06-22 | 山东省鲁洲食品集团有限公司 | Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues |
| CN102102116B (en) * | 2010-12-21 | 2013-01-02 | 山东省鲁洲食品集团有限公司 | Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues |
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