CN102559804A - Method for preparing high-purity XOS by adopting straw and rice husk - Google Patents

Method for preparing high-purity XOS by adopting straw and rice husk Download PDF

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CN102559804A
CN102559804A CN2010105921086A CN201010592108A CN102559804A CN 102559804 A CN102559804 A CN 102559804A CN 2010105921086 A CN2010105921086 A CN 2010105921086A CN 201010592108 A CN201010592108 A CN 201010592108A CN 102559804 A CN102559804 A CN 102559804A
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solution
rice husk
straw
xylooligosaccharides
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历冠廷
胡国华
徐金矿
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Suzhou Industrial Park Shangrong Technology Co Ltd
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Suzhou Industrial Park Shangrong Technology Co Ltd
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Abstract

The invention relates to a method for preparing high-purity XOS by adopting straw and rice husk. The invention adopts the technology as follows: grinding 50 to 70% of straw and 30 to 50% of rice husk to be soaked by hot water and filtered; adding NaOH water solution for alkaline treatment; centrifugally obtaining extraction solution to be neutralized by acetic acid water solution; centrifugally removing sediment and concentrating supernate to be on sediment and standing through ethanol; centrifugally collecting sediment, drying the sediment to remove the ethanol and mixing the sediment into water solution; performing enzymolysis treatment on complex enzyme water solution; performing inactivation on the enzymolysis solution for vacuum concentration after the enzymolysis treatment; utilizing large adsorptive cationic resin to purify the concentrated solution, vacuum drying to obtain yellow-white particle XOS, and throwing the powdered XOS into a spraying fluid bed, so as to enable the material to flow from the bottom of the bed into the bed under the positive pressure and flow from bottom to top in an accelerating way and the XOS solution to be continuously sprayed and scattered onto the XOS, therefore, dry fluffy particle high-purify XOS is obtained.

Description

A kind of method that adopts straw and rice husk to prepare high-purity oligoxylose
Technical field
The present invention relates to the method that a kind of straw and rice husk prepare high-purity oligoxylose.
Background technology
Xylooligosaccharides is also claimed wood oligose; Be a kind of important function property food; Except having low-heat, good physicochemical characteristics such as stable, safe, nontoxic, also have the breeding that promotes probiotics in the enteron aisle, the unique physiological function that suppresses harmful bacteria growing, caused global extensive concern at present.At present the preparation xylooligosaccharides is to be raw material with cellulosic materials such as corn cob, bagasse mostly; With the straw is that the feedstock production xylooligosaccharides still belongs to blank.
Yet, the several hundred million tons of China's straw and rice husk YO, straw and rice husk account for about 70% of paddy by weight, are the main sub products at rice rice mill and paddy rice plantation family.The present application of straw and rice husk mainly concentrates on conventional use, like animal-feed, paper making raw material and infertile field etc., does not have more effective development and use; Traditional method is that straw and rice husk are burned in a large number in the rural area, produces a large amount of greenhouse gases, havoc the ecotope balance, cause exhaustion of soil, quickened the vicious cycle on the agricultural, polluted environment, especially the hidden danger of fire.The development and use purposes of straw and rice husk does not seldom all really form industrial scaleization.
If can be the feedstock production xylooligosaccharides with straw and rice husk, straw and rice husk are turned waste into wealth, have great economic worth, and solved problems such as the wasting of resources and environmental pollution.Therefore; The market in urgent need exploitation is a kind of to be the method for feedstock production xylooligosaccharides with straw and rice husk; Especially be badly in need of a kind of low cost of research, consistent, high purity, simple to operate, pollution-free and what be suitable for large-scale production is the method for feedstock production high-purity oligoxylose with straw and rice husk; For development of agricultural products turns waste into wealth straw and rice husk, promote high added value and open up the new market of a slice, for the mankind provide a kind of high-touch feature Sexual health sugar products kind.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of method that adopts straw and rice husk to prepare high-purity oligoxylose is provided.
The object of the invention is realized through following technical scheme:
A kind of method that adopts straw and rice husk to prepare high-purity oligoxylose is characterized in that may further comprise the steps:
1. take by weighing straw, rice husk, wherein straw 50%~70%, and rice husk 30%~50% is pulverized straw, rice husk, handles with hot-water soak, filters, and discards filtrating;
2. add the NaOH aqueous solution and carry out alkaline purification, its alkali purification temp is 30~55 ℃, and the alkaline purification time is 26~34 hours;
3. centrifugal acquisition extracting solution is used the acetic acid aqueous solution neutralising extract, to pH be 5.0~7.0;
4. centrifugal removal deposition after supernatant concentration, is used ethanol sedimentation, leaves standstill then;
5. centrifugal collecting precipitation, dry sediment is made into throw out 4~5% the aqueous solution then to remove ethanol wherein;
6. prozyme is carried out enzymolysis processing to the aqueous solution that 5. step makes in proportion, hydrolysis temperature is 30~40 ℃, and enzymolysis time is 25~33 hours, adds 0.1~4g prozyme in the 100mL treating water solution; The component of wherein said prozyme is: endo-xylanase 40~60wt%, arabinofuranosidase 20~35wt%, circumscribed zytase 15~35wt%;
7. after enzymolysis finishes, with enzymolysis solution in 105~120 ℃ of deactivations 10~15 minutes, then in 45~60 ℃ of vacuum concentration;
8. with macroporous type absorption resin cation(R.C.) purifying liquid concentrator; Be about to resin and fully moisten and rise, press the consumption of the concentrated complex enzyme hydrolysis liquid of 100g resin 200mL, 25~39 ℃ of following adsorption treatment 10~21 hours; Filter then; With 30~45% ethanolic soln wash-outs, after elutriant concentrates earlier, the desalination in 20~60 hours of dialysing again; In 46~53 ℃ of vacuum-dryings 15~18 hours, obtain light yellow then to white powdered granule xylooligosaccharides;
9. the powdered granule xylooligosaccharides 5~10% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 90~95% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body; Spraying drying obtains the fluffy granular high-purity oligoxylose continuously.
Further, above-mentioned a kind of method that adopts straw and rice husk to prepare high-purity oligoxylose, 1. said the processing with hot-water soak of step is meant with 55~60 ℃ of hot-water soaks 5~10 hours.The concentration of the 2. said NaOH aqueous solution of step is 0.8~4%, uses volume 30~55 times as straw and rice husk weight.The step 3. concentration of said acetic acid aqueous solution is 30~50%.
Substantive distinguishing features and obvious improvement that technical scheme of the present invention is outstanding are mainly reflected in:
The invention provides low cost, high purity, easy to operate simple, pollution-free and be suitable for the method for preparing high-purity oligoxylose of large-scale production; Prepare through the complex enzyme zymohydrolysis technology with straw and rice husk; The negative pressure fluidized-bed fluidization technique of uses advanced combines the multi-point atomizing method; Time sharing segment opertaing device bed temperature efficiently solves homodisperse, coats problems such as granulation, drying.With agriculture byproduct straw and rice husk is raw material, employs new technology, novel method promotes and raise the efficiency, and straw is turned waste into wealth open up new markets and frontier.Its preparation process science is simple and easy to operate, is fit to very much large-scale production.
Embodiment
The present invention provides a kind of low cost, high purity, easy to operate simple, pollution-free and be suitable for large-scale production prepares high-purity oligoxylose through the complex enzyme zymohydrolysis technology with straw and rice husk method; Employ new technology, novel method raises the efficiency; Straw and rice husk are turned waste into wealth, open up new market and new field.
The preparation method of high-purity oligoxylose pulverizes with each 50%~70% straw and 30%~50% rice husk, and through complex enzyme zymohydrolysis technology preparation high-purity oligoxylose, concrete steps are:
1. take by weighing the straw and the rice husk of ratio, straw, rice husk are pulverized,, filter, discard filtrating with 55~60 ℃ of hot-water soaks 5~10 hours;
2. add the NaOH aqueous solution and carry out alkaline purification, the concentration of the NaOH aqueous solution is 0.8~4%, uses volume 30~55 times as straw weight, and its alkali purification temp is 30~55 ℃, and the alkaline purification time is 26~34 hours;
3. centrifugal acquisition extracting solution, using the acetic acid aqueous solution neutralising extract is 5.0~7.0 to pH, the concentration of acetic acid aqueous solution is 30~50%;
4. centrifugal removal deposition after supernatant concentration, is used ethanol sedimentation, and alcohol concn is 95%, leaves standstill then 7~10 hours;
5. centrifugal collecting precipitation, dry sediment is made into throw out 4~5% the aqueous solution then to remove ethanol wherein;
6. prozyme is carried out enzymolysis processing to the aqueous solution that 5. step makes in proportion, hydrolysis temperature is 30~40 ℃, and enzymolysis time is 25~33 hours, adds 0.1~4g prozyme in the 100mL treating water solution; Wherein, the component of prozyme is: endo-xylanase 40~60wt%, arabinofuranosidase 20~35wt%, circumscribed zytase 15~35wt%;
7. after enzymolysis finishes, with enzymolysis solution in 105~120 ℃ of deactivations 10~15 minutes, then in 45~60 ℃ of vacuum concentration;
8. with macroporous type absorption resin cation(R.C.) purifying liquid concentrator; Promptly earlier resin is fully moistened and rise, press the consumption of the concentrated complex enzyme hydrolysis liquid of 100g resin 200mL, 25~39 ℃ of following adsorption treatment 10~21 hours; Filter then; With 30~45% ethanolic soln wash-outs, after elutriant concentrates earlier, the desalination in 20~60 hours of dialysing again; In 46~53 ℃ of vacuum-dryings 15~18 hours, obtain light yellow then to white powdered granule xylooligosaccharides;
9. the powdered granule xylooligosaccharides 5~10% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 90~95% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body; Spraying drying obtains the fluffy granular high-purity oligoxylose continuously.
Embodiment 1
Take by weighing straw 70%, rice husk 30% in proportion, straw segment and rice husk are pulverized together, steeped 8 hours, filter, discard filtrating with 51 ℃ of water loggings; The concentration that is incorporated as straw and 45 times of volumes of rice husk weight was 4% the NaOH aqueous solution, 50 ℃ of following alkaline purifications 30 hours; Centrifugal extracting solution, to use concentration be 31% acetate neutralising extract to pH be 5.0; Centrifugal removal precipitates, and after above-mentioned clear liquid is concentrated, uses 95% ethanol sedimentation, and used 95% alcoholic acid volume is 3 times of liquid concentrator volume; Left standstill 7 hours; Centrifugal collecting precipitation, dry sediment is made into throw out 4% the aqueous solution then to remove ethanol wherein; Add prozyme (prozyme contains endo-xylanase, arabinofuranosidase, circumscribed zytase, and ratio is 45: 20: 35), the prozyme that wherein adds 0.15g in the 100mL treating water solution carried out enzymolysis processing 32 hours at 38 ℃ to the aqueous solution; With enzymolysis solution in 117 ℃ of deactivations 12 minutes, then in 50 ℃ of vacuum concentration; With macroporous type absorption resin cation(R.C.) purifying liquid concentrator: promptly earlier resin is fully moistened and rise, press the consumption of the concentrated enzymolysis solution of 100g resin 200mL, 28 ℃ of following adsorption treatment 15 hours; Filter then; With 45% ethanolic soln wash-out, after elutriant concentrates earlier, the desalination in 60 hours of dialysing again; In 50 ℃ of vacuum-dryings 15 hours, obtain light yellow at last to white powdered granule xylooligosaccharides; Obtain xylooligosaccharides purity and be 80%, 20% other be hemicellulose B and wood sugar.Then the powdered granule xylooligosaccharides 10% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 90% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body, and spraying drying obtains the fluffy granular high-purity oligoxylose continuously.Xylooligosaccharides purity is 80%.
Embodiment 2
Take by weighing straw 65%, rice husk 35% in proportion, straw and rice husk are pulverized together, steeped 9 hours, filter, discard filtrating with 52 ℃ of water loggings; The concentration that is incorporated as straw and 47 times of volumes of rice husk weight was 2.5% the NaOH aqueous solution, 52 ℃ of following alkaline purifications 30 hours; Centrifugal extracting solution, to use concentration be 32% acetate neutralising extract to pH be 5.0; Centrifugal removal deposition after supernatant concentration, is used 95% ethanol sedimentation, and used 95% alcoholic acid volume is 4 times of liquid concentrator volume; Left standstill 7 hours; Centrifugal collecting precipitation, dry sediment is made into throw out 4.5% the aqueous solution then to remove ethanol wherein; (prozyme contains endo-xylanase, arabinofuranosidase, circumscribed zytase to add prozyme; Ratio is (40: 30: 30); Wherein carry out enzymolysis processing 33 hours with prozyme at 36 ℃ of aqueous solution in the 100mL treating water solution, wherein add the 0.15g prozyme in the 100mL treating water solution; With enzymolysis solution in 119 ℃ of deactivations 13 minutes, then in 55 ℃ of vacuum concentration; With macroporous type absorption resin cation(R.C.) purifying liquid concentrator: at first resin is fully moistened and rise, press the consumption of the concentrated enzymolysis solution of 100g resin 200mL, 30 ℃ of following adsorption treatment 16 hours; Filter then; With 43% ethanolic soln wash-out, after elutriant concentrates earlier, the desalination in 64 hours of dialysing again; In 55 ℃ of vacuum-dryings 16 hours, obtain light yellow at last to white powdered granule xylooligosaccharides; Obtain xylooligosaccharides purity and be 81%, 19% other be hemicellulose B and wood sugar.Then the powdered granule xylooligosaccharides 5% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 95% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body, and spraying drying obtains the fluffy granular high-purity oligoxylose continuously.Xylooligosaccharides purity is 81%.
Embodiment 3
Take by weighing straw 60%, rice husk 40% in proportion, straw and rice husk are pulverized together, steeped 11 hours, filter, discard filtrating with 50 ℃ of water loggings; The concentration that is incorporated as straw and 50 times of volumes of rice husk weight was 1.5% the NaOH aqueous solution, 54 ℃ of following alkaline purifications 32 hours; Centrifugal extracting solution, to use concentration be 30% acetate neutralising extract to pH be 5.5; Centrifugal removal deposition after supernatant concentration, is used 95% ethanol sedimentation, and used 95% alcoholic acid volume is 4 times of liquid concentrator volume; Left standstill 8 hours; Centrifugal collecting precipitation, dry sediment is made into throw out 5% the aqueous solution then to remove ethanol wherein; Add prozyme (contain endo-xylanase, arabinofuranosidase, circumscribed zytase, ratio is 50: 35: 15), at 37 ℃ the aqueous solution was carried out enzymolysis processing 36 hours, wherein add the 0.2g prozyme in the 100mL treating water solution with prozyme; With enzymolysis solution in 118 ℃ of deactivations 14 minutes, then in 56 ℃ of vacuum concentration; With macroporous type absorption resin cation(R.C.) purifying liquid concentrator: promptly earlier resin is fully moistened and rise, press the consumption of the concentrated enzymolysis solution of 100g resin 200mL, 20 ℃ of following adsorption treatment 20 hours; Filter then; With 42% ethanolic soln wash-out, after elutriant concentrates earlier, the desalination in 66 hours of dialysing again; In 45 ℃ of vacuum-dryings 17 hours, obtain light yellow at last to white powdered granule xylooligosaccharides; Obtain xylooligosaccharides purity and be 82%, 18% other be hemicellulose B and wood sugar.Then the powdered granule xylooligosaccharides 8% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 92% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body, and spraying drying obtains the fluffy granular high-purity oligoxylose continuously.Xylooligosaccharides purity is 82%.
Embodiment 4
Take by weighing straw 500%, rice husk 50% in proportion, straw and rice husk are pulverized together, steeped 6 hours, filter, discard filtrating with 56 ℃ of water loggings; The concentration that is incorporated as straw and 60 times of volumes of rice husk weight was 2.0% the NaOH aqueous solution, 55 ℃ of following alkaline purifications 34 hours; Centrifugal extracting solution, to use concentration be 35% acetate neutralising extract to pH be 6.0; Centrifugal removal deposition after supernatant concentration, is used 95% ethanol sedimentation, and used 95% alcoholic acid volume is 4 times of liquid concentrator volume, leaves standstill 10 hours; Centrifugal collecting precipitation, dry sediment is made into throw out 5% the aqueous solution then to remove ethanol wherein; Add prozyme (contain endo-xylanase, arabinofuranosidase, circumscribed zytase, ratio is 55: 25: 20), at 40 ℃ the aqueous solution was carried out enzymolysis processing 24 hours, wherein add the 0.25g prozyme in the 100mL treating water solution with prozyme; With enzymolysis solution in 120 ℃ of deactivations 15 minutes, then in 60 ℃ of vacuum concentration; With macroporous type absorption resin cation(R.C.) purifying liquid concentrator: promptly earlier resin is fully moistened and rise, press the consumption of the concentrated enzymolysis solution of 100g resin 200mL, 35 ℃ of following adsorption treatment 10 hours; Filter then; With 45% ethanolic soln wash-out, after elutriant concentrates earlier, the desalination in 72 hours of dialysing again; At last in 53 ℃ of vacuum-dryings 18 hours,, obtain light yellow to white powdered granule xylooligosaccharides; Obtain xylooligosaccharides purity and be 85%, 15% other be hemicellulose B and wood sugar.Then the powdered granule xylooligosaccharides 6% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 94% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body, and spraying drying obtains the fluffy granular high-purity oligoxylose continuously.Xylooligosaccharides purity is 85%.
Embodiment 5
Take by weighing straw 55%, rice husk 45% in proportion, straw segment and rice husk are pulverized together, steeped 10 hours, filter, discard filtrating with 54 ℃ of water loggings; The concentration that is incorporated as straw and 30 times of volumes of rice husk weight was 0.8% the NaOH aqueous solution, 30 ℃ of following alkaline purifications 26 hours; Centrifugal extracting solution, to use concentration be 34% acetate neutralising extract to pH be 7.0; Centrifugal removal precipitates, and after above-mentioned clear liquid is concentrated, uses 95% ethanol sedimentation, and used 95% alcoholic acid volume is 5 times of liquid concentrator volume; Left standstill 8 hours; Centrifugal collecting precipitation, dry sediment is made into throw out 4.5% the aqueous solution then to remove ethanol wherein; Add prozyme (prozyme contains endo-xylanase, arabinofuranosidase, circumscribed zytase, and ratio is 60: 25: 15), the prozyme that wherein adds 0.2g in the 100mL treating water solution carried out enzymolysis processing 25 hours at 40 ℃ to the aqueous solution; With enzymolysis solution in 120 ℃ of deactivations 14 minutes, then in 40 ℃ of vacuum concentration; With macroporous type absorption resin cation(R.C.) purifying liquid concentrator: promptly earlier resin is fully moistened and rise, press the consumption of the concentrated enzymolysis solution of 100g resin 200mL, 25 ℃ of following adsorption treatment 12 hours; Filter then; With 40% ethanolic soln wash-out, after elutriant concentrates earlier, the desalination in 50 hours of dialysing again; In 46 ℃ of vacuum-dryings 14 hours, obtain light yellow at last to white powdered granule xylooligosaccharides; Obtain xylooligosaccharides purity and be 83%, 17% other be hemicellulose B and wood sugar.Then the powdered granule xylooligosaccharides 7% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 93% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body, and spraying drying obtains the fluffy granular high-purity oligoxylose continuously.Xylooligosaccharides purity is 83%.
Through detecting, adopt the fluffy granular high-purity oligoxylose of technical scheme acquisition of the present invention, its main performance index is seen table 1.
Table 1
Figure BSA00000388459200091
In sum, the present invention adopts advanced science and technology technology and method, adopts agriculture byproduct to prepare high-purity oligoxylose, and the output high added value is fit to large-scale production very much, is worth wide popularization and application in the field of business.
What need understand is: the above only is a preferred implementation of the present invention; For those skilled in the art; Under the prerequisite that does not break away from the principle of the invention, can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.

Claims (4)

1. method that adopts straw and rice husk to prepare high-purity oligoxylose is characterized in that may further comprise the steps:
1. take by weighing straw, rice husk, wherein straw 50%~70%, and rice husk 30%~50% is pulverized straw, rice husk, handles with hot-water soak, filters, and discards filtrating;
2. add the NaOH aqueous solution and carry out alkaline purification, its alkali purification temp is 30~55 ℃, and the alkaline purification time is 26~34 hours;
3. centrifugal acquisition extracting solution is used the acetic acid aqueous solution neutralising extract, to pH be 5.0~7.0;
4. centrifugal removal deposition after supernatant concentration, is used ethanol sedimentation, leaves standstill then;
5. centrifugal collecting precipitation, dry sediment is made into throw out 4~5% the aqueous solution then to remove ethanol wherein;
6. prozyme is carried out enzymolysis processing to the aqueous solution that 5. step makes in proportion, hydrolysis temperature is 30~40 ℃, and enzymolysis time is 25~33 hours, adds 0.1~4g prozyme in the 100mL treating water solution; The component of wherein said prozyme is: endo-xylanase 40~60wt%, arabinofuranosidase 20~35wt%, circumscribed zytase 15~35wt%;
7. after enzymolysis finishes, with enzymolysis solution in 105~120 ℃ of deactivations 10~15 minutes, then in 45~60 ℃ of vacuum concentration;
8. with macroporous type absorption resin cation(R.C.) purifying liquid concentrator; Be about to resin and fully moisten and rise, press the consumption of the concentrated complex enzyme hydrolysis liquid of 100g resin 200mL, 25~39 ℃ of following adsorption treatment 10~21 hours; Filter then; With 30~45% ethanolic soln wash-outs, after elutriant concentrates earlier, the desalination in 20~60 hours of dialysing again; In 46~53 ℃ of vacuum-dryings 15~18 hours, obtain light yellow then to white powdered granule xylooligosaccharides;
9. the powdered granule xylooligosaccharides 5~10% that obtains is joined in the heating container, add deionized water and mix, rising temperature for dissolving adds gac in the solution, filtered while hot, and filtrating is pooled in the storage tank, obtains xylooligosaccharides solution; The powdered granule xylooligosaccharides 90~95% that obtains is put in the spray-fluidized bed apparatus; Material also quickens to flow from the bottom entering fluidized bed with spraying of fluidized bed with spraying with malleation from bottom to top; The top of fluidized bed with spraying impose negative pressure vibrate from top to bottom make material in fluidized-bed up and down the boiling; Multiple spot spray gun by the fluidized-bed sidepiece is distributed to the continuous spraying of the above-mentioned xylooligosaccharides solution that refines on the fine xylooligosaccharides body; Spraying drying obtains the fluffy granular high-purity oligoxylose continuously.
2. a kind of method that adopts straw and rice husk to prepare high-purity oligoxylose according to claim 1 is characterized in that: 1. said the processing with hot-water soak of step is meant with 55~60 ℃ of hot-water soaks 5~10 hours.
3. a kind of method that adopts straw and rice husk to prepare high-purity oligoxylose according to claim 1 is characterized in that: the concentration of the 2. said NaOH aqueous solution of step is 0.8~4%, uses volume 30~55 times as straw and rice husk weight.
4. a kind of method that adopts straw and rice husk to prepare high-purity oligoxylose according to claim 1 is characterized in that: the step 3. concentration of said acetic acid aqueous solution is 30~50%.
CN2010105921086A 2010-12-16 2010-12-16 Method for preparing high-purity XOS by adopting straw and rice husk Pending CN102559804A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN104631168A (en) * 2015-01-28 2015-05-20 广西壮族自治区中国科学院广西植物研究所 Application of wet stacking in keeping hemicellulose with macromolecular structure characteristics in straw and straw storage method
CN105161155A (en) * 2015-08-10 2015-12-16 南华大学 Method absorbing and processing uranium-bearing waste water via sodium hydroxide modified rice straw absorbent
CN105463040A (en) * 2016-01-13 2016-04-06 中国科学院过程工程研究所 Method for raising yield of xylooligosaccharide
CN105483184A (en) * 2016-01-07 2016-04-13 中国科学院过程工程研究所 Production method of high-yield xylooligosaccharide

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Application publication date: 20120711