CN106498001A - A kind of improved clean manufacturing xylose process - Google Patents
A kind of improved clean manufacturing xylose process Download PDFInfo
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- CN106498001A CN106498001A CN201610904859.4A CN201610904859A CN106498001A CN 106498001 A CN106498001 A CN 106498001A CN 201610904859 A CN201610904859 A CN 201610904859A CN 106498001 A CN106498001 A CN 106498001A
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
Abstract
The invention discloses a kind of improved clean manufacturing xylose process, the processing technology be by agriculture and forestry organic waste material by pretreatment of raw material digest separation of solid and liquid concentrate pre- decolouring chromatographic isolation refined after, the final refined and crystallization for obtaining wood sugar and arabinose refined and crystallize.The present invention has the advantages that：Steam explosion temperature is relatively low, and steam explosion technique realizes continuous prodution；Xylan in raw material is converted into the conversion ratio of wood sugar and reaches more than 95%；Further such that the impurity in liquid glucose reduces the steam explosion time greatly shortening, water consume is reduced, and protects chromatographic isolation resin, extends the service life of resin, has effectively saved steam, reduces steam explosion cost.
Description
Technical field
The present invention relates to the production technical field of wood sugar, specifically a kind of improved clean manufacturing xylose process.
Background technology
Traditional xylose production process is acid hydrolysis process, specifically will be enriched in the agriculture and forestry organic waste material of hemicellulose（Such as jade
Meter Xin, bagasse, bamboo, birch-bark, straw）Carry out decolourizing after sour water solution, desalination, after the refined purification of step such as concentration
Crystallization, centrifugation obtain crystal wood sugar.In this technique, sulfate ion content is higher, and desalination operation soda acid consumption is big, and water consumption is big,
It is the main source of sewage in xylose production, while the activity of the anaerobic bacteria that sulfuric acid can be in inhibitory activity sludge.
The patent of Patent No. 201410701716.4《A kind of technique of clean manufacturing wood sugar》In refer to similar enzyme process
The production technology of wood sugar is prepared, and the present invention is that following improvement is made that on the basis of the patent：1st, continuous steam explosion technology is adopted,
Realize that serialization feeds intake；2nd, reduce steaming quick-fried temperature, reduce the degraded of cellulose, improve xylose purity；3rd, after concentrating, color is carried out
Spectrum is separated, and improving efficiency reduces water consume；4th, enzyme system of the enzymolysis using multiple enzymes composition, improves enzymolysis efficiency；5th, before chromatographic isolation
Pre- decolorization process is added, chromatogram separation resin is protected.6th, chromatographic isolation adopts three phase separation, and arabinose is separated.
The patent of Patent No. 200610040383.0《The enzymatic-process preparation method of wood sugar》In describe similar approach, but deposit
In following deficiency：1st, the pretreatment described in the method refers to that alkali carries take or steam explosion, and unspecified specific process parameter, different
Steam explosion equipment, the liquid glucose component difference obtained by condition directly affect the addition of enzyme, be consequently belonging to insufficient disclosure；2nd, enzyme
Solution insufficient, by patent description of the drawings 2-6 in as can be seen that enzymolysis after liquid glucose in containing substantial amounts of xylan and other not
The miscellaneous sugar that indicates, xylose purity is less than 50%, it is commonly known that the crystallization purity of wood sugar needs to reach more than 75%.3rd, heavy using ethanol
Shallow lake impurity, ethanol are relatively costly, and operating environment is poor, go that removal of impurity effect is not obvious, and industrialized production is uneconomical.
The patent of Patent No. 200510045325.2《A kind of method of Production by Enzymes wood sugar》In refer to similar technique,
But have the following disadvantages：1st, the pretreatment described in the method refers to autoclaving or steam explosion, and gives autoclaving condition, so
And the string hemicellulose after autoclaving is unstripped out, it is unfavorable for the infiltration of enzyme, inefficiency；The patent is not carried
To the specific technological parameter of steam explosion and device type, belong to insufficient disclosure；2nd, described enzyme refers to circumscribed-type zytase, and
Technically single circumscribed-type zytase efficiency is low, needs and other enzyme collective effects；3rd, the wood that mentions in patent gathers
The conversion ratio of sugar conversion wood sugar reaches more than 80%, does not have advance, and traditional sulphuric acid hydrolysis conversion ratio is more than 85%.
Patent No. 201110162361.2《A kind of production technology for preparing wood sugar and L-arabinose of clean and effective》
Patent mention similar technique, but have the following disadvantages：1st, the enzymolysis enzyme is aspergillus niger crude enzyme liquid, complicated component efficiency
Low, high cost is refined, selectivity is not high；2nd, the thermophilic digestion described in the method gives autoclaving condition, but reaction time
Longer, side reaction is more, and in the string after thermophilic digestion, hemicellulose is separated without steam explosion, is unfavorable for oozing for enzyme or microorganism
Enter, enzymolysis efficiency is low.
Content of the invention
The technical assignment of the present invention is to provide a kind of improved clean manufacturing xylose process.
The technical assignment of the present invention realizes that the xylose production process step is as follows in the following manner：
1）Pretreatment of raw material：Steam explosion equipment is warming up to 120 DEG C -160 DEG C in advance, agriculture and forestry organic waste material is put into steam explosion equipment then
In, agriculture and forestry organic waste material holdup time in steam explosion equipment is 5min-60min, and 120 DEG C -160 DEG C of steam explosion temperature, every 2s spurt one
Secondary material using mechanical steam recompression device by the Steam Recovery that isolates, and is circulated and is passed through steam explosion to cyclone separator
Equipment steam inlet, through steam explosion after agriculture and forestry organic waste material import enzymatic vessel；
2）Enzymolysis：With the material dry matter content in pure water regulation enzymatic vessel to mass percent 10%-30%, and pH value is adjusted to 3.0-
5.7,40 DEG C -57 DEG C of control system temperature, by 1 ‰ -5 ‰ addition enzyme systems of raw material amount of dry matter, is incubated 10-30h；
3）Separation of solid and liquid：Material plate-frame filtering after by enzymolysis, obtains filtered fluid, and drip washing Production With Residue of Enzymatic Hydrolysis 2-3 time, obtains drip washing
Liquid, obtains enzymolysis liquid with filtered fluid after leacheate is mixed；
4）Concentration：Enzymolysis liquid is concentrated to dryness amount of substance content 30%-50%, concentrate is obtained；
5）Pre- decolouring：The activated carbon that amount of dry matter content adds 1%-2% is pressed in concentrate, at 60-80 DEG C is incubated 30-60min,
It is filtrated to get destainer；
6）Chromatographic isolation is refined：Using three-phase chromatographic separation technology, destainer is separated into by miscellaneous liquid, wood by chromatographic isolation resin
Liquid glucose, three components of Arabic liquid glucose；
7）The refined and crystallization of wood sugar：The Xylose that chromatographic isolation is obtained is crossed cation and anion exchange resin, residual impurity is removed
Ion, obtains wood sugar refined liquid, and concentrated, crystallization, centrifugation obtain xylose crystals；
8）The refined and crystallization of arabinose：The Arabic liquid glucose that chromatographic isolation is obtained is crossed cation and anion exchange resin, is removed
Residual impurity ion, obtains arabinose refined liquid, and concentrated, crystallization, centrifugation obtain arabinose crystal
Described agriculture and forestry organic waste material is corncob, bagasse, the one kind in birch-bark.
Described step 2）Middle enzyme system is by β-Isosorbide-5-Nitrae-endo-xylanase, xylobiase, α-L- furan type arabinoses
Glycosides enzyme, phlorose aldehyde neuraminidase, phenolic aldehyde esterase are constituted, and the weight of each constituent is as follows：β -1,4- inscribes wood is poly-
Carbohydrase 1-2 parts, xylobiase 0.5-1 parts, α-L- furan type arabinosidase 0.5-1 parts, phlorose aldehyde neuraminidase
0.5-1 parts, phenolic aldehyde esterase 0.3-0.5 parts.
Described chromatographic isolation resin is the one kind in sodium form, potassium type, calcium type and Hydrogen chromatographic isolation resin.
Described step 1）Before in the middle input steam explosion equipment by agriculture and forestry organic waste material, need continuously to put into after water is cleaned
After in steam explosion equipment or agriculture and forestry organic waste material being put into steam explosion equipment feed well and is soaked with dilute sulfuric acid in input steam explosion equipment.
The mass percent concentration of described dilute sulfuric acid is 0.1%-0.5%.
Compared to the prior art the clean manufacturing xylose process of a modification of the present invention, has the advantages that：
1）Steam explosion temperature is relatively low, and steam explosion technique realizes continuous prodution；Hemicellulose in agriculture and forestry organic waste material big portion after steam explosion
Divide and be degraded to monose and compound sugar, cellulose degradation is less, and therefore glucose and beta-dextran content are relatively low in soluble sugar, about
5% or so, the xylan in raw material is converted into the conversion ratio of wood sugar and reaches more than 95%；
2）Agriculture and forestry organic waste material is cleaned the attachment for being effectively reduced impurity for a time with water, further such that miscellaneous in liquid glucose before steam explosion
Matter is reduced.
3）Compared with traditional wood sugar hydrolysis method, the steam explosion time greatly shortens, the stripping of hemicellulose, cellulose and lignin
Larger from degree, be conducive to the carrying out for digesting.
4）The enzyme system combined using multiple enzymes, enzymolysis efficiency are higher, and glycan is degradable into monose, the glycan of residual
Content is less than 1%.
5）Concentration and pre- decolouring is first carried out before chromatrographic separation step, is improved the concentration of sugar in feed liquid, is made chromatographic isolation efficiency
Improve, water consume is reduced, protect chromatographic isolation resin, extend the service life of resin.Three phase separation technology is adopted simultaneously, will be miscellaneous
Matter, wood sugar, arabinose are separated, and are reduced the impurity content in liquid glucose and are respectively obtained wood sugar and arabinose.
6）Using mechanical steam recompression device by the Steam Recovery that isolates, steam is effectively saved, reduced vapour
Burst into this.
Specific embodiment
Configuration enzyme system is standby：Enzyme system constituent weight be β-Isosorbide-5-Nitrae-endo-xylanase 1-2 parts, β-xyloside
Enzyme 0.5-1 parts, α-L- furan type arabinosidase 0.5-1 parts, phlorose aldehyde neuraminidase 0.5-1 parts, phenolic aldehyde esterase 0.3-
0.5 part；
Preferred β -1 part of Isosorbide-5-Nitrae-endo-xylanase, 0.5 part of xylobiase, 0.5 part of α-L- furan types arabinosidase,
0.5 part of phlorose aldehyde neuraminidase, 0.3 part of phenolic aldehyde esterase.
Embodiment 1：
1）Pretreatment of raw material：Steam explosion equipment is warming up to 120 DEG C in advance, puts into steam explosion equipment by continuous after water cleaning for bagasse
In, the material lagging time is 60min, and 120 DEG C of steam explosion temperature, every 2s spurt material to cyclone separator, using mechanical steam
Recompression device is by the Steam Recovery that isolates, and circulates and be passed through steam explosion equipment steam inlet, through steam explosion after agriculture and forestry organic waste material
Import enzymatic vessel；
2）Enzymolysis：Material dry matter content in enzymatic vessel is adjusted to 30% with pure water, and pH value is adjusted to 5.7, control system temperature 57
DEG C, by 5 ‰ addition enzyme systems of raw material amount of dry matter, it is incubated 10h；
3）Separation of solid and liquid：Material plate-frame filtering after by enzymolysis, obtains filtered fluid, and drip washing Production With Residue of Enzymatic Hydrolysis 3 times, makes the overwhelming majority
Sugar be dissolved out, obtain leacheate, after leacheate is mixed with filtered fluid, obtain enzymolysis liquid；The now grape in enzymolysis liquid
Sugared purity is 4.8%, and it is 95.4% that the xylan in raw material is converted into the conversion ratio of wood sugar.
4）Concentration：Enzymolysis liquid is concentrated into dry matter content 50% with evaporimeter, concentrate is obtained；
5）Pre- decolouring：The activated carbon that dry matter content adds 2% is pressed in concentrate, is incubated 60min, is filtrated to get decolouring at 80 DEG C
Liquid；
6）Chromatographic isolation is refined：Using three-phase chromatographic separation technology, using calcium type separation resin, by destainer be separated into miscellaneous liquid,
Xylose, three components of Arabic liquid glucose；
7）The refined and crystallization of wood sugar：The Xylose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove residual impurity ion,
Wood sugar refined liquid is obtained, concentrated, crystallization, centrifugation obtain xylose crystals；
8）The refined and crystallization of arabinose：The Arabic liquid glucose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove remaining
Foreign ion, obtains arabinose refined liquid, and concentrated, crystallization, centrifugation obtain arabinose crystal.
Embodiment 2：
1）Pretreatment of raw material：Steam explosion equipment is warming up to 160 DEG C in advance, by the corncob dilute sulfuric acid of mass percent concentration 0.5%
After solution immersion 5h in continuous input steam explosion equipment, the material lagging time is 5min, and 160 DEG C of steam explosion temperature, every 2s spurt material
To cyclone separator, using mechanical steam recompression device by the Steam Recovery that isolates, and circulate be passed through steam explosion equipment steaming
Vapour entrance, through steam explosion after agriculture and forestry organic waste material import enzymatic vessel；
2）Enzymolysis：Material dry matter content in enzymatic vessel is adjusted to 10% with pure water, and pH value is adjusted to 3.0, control system temperature 40
DEG C, by 1 ‰ addition enzyme systems of raw material amount of dry matter, it is incubated 30h；
3）Separation of solid and liquid：Material plate-frame filtering after by enzymolysis, obtains filtered fluid, and drip washing Production With Residue of Enzymatic Hydrolysis 2 times, makes the overwhelming majority
Sugar be dissolved out, obtain leacheate, after leacheate is mixed with filtered fluid, obtain enzymolysis liquid；The now grape in enzymolysis liquid
Sugared purity is 3.4%, and it is 98.3% that the xylan in raw material is converted into the conversion ratio of wood sugar；
4）Concentration：Enzymolysis liquid is concentrated into dry matter content 30% with evaporimeter, concentrate is obtained；
5）Pre- decolouring：The activated carbon that dry matter content adds 1% is pressed in concentrate, is incubated 30min, is filtrated to get decolouring at 60 DEG C
Liquid；
6）Chromatographic isolation is refined：Using three-phase chromatographic separation technology, using sodium form separation resin, by destainer be separated into miscellaneous liquid,
Xylose, three components of Arabic liquid glucose；
7）The refined and crystallization of wood sugar：The Xylose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove residual impurity ion,
Wood sugar refined liquid is obtained, concentrated, crystallization, centrifugation obtain xylose crystals；
8）The refined and crystallization of arabinose：The Arabic liquid glucose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove remaining
Foreign ion, obtains arabinose refined liquid, and concentrated, crystallization, centrifugation obtain arabinose crystal.
Embodiment 3
1）Pretreatment of raw material：Steam explosion equipment is warming up to 140 DEG C in advance, will connect after dilution heat of sulfuric acid immersion 5h of the birch-bark with 0.2%
In continuous input steam explosion equipment, the material lagging time is 8min, and 140 DEG C of steam explosion temperature spurts material to cyclone separator per 2s, sharp
With mechanical steam recompression device by the Steam Recovery that isolates, and circulate and be passed through steam explosion equipment steam inlet, through steam explosion after
Agriculture and forestry organic waste material import enzymatic vessel；
2）Enzymolysis：Material dry matter content in enzymatic vessel is adjusted to 20% with pure water, and pH value is adjusted to 5.5, control system temperature 50
DEG C, by 2 ‰ addition enzyme systems of raw material amount of dry matter, it is incubated 24h；
3）Separation of solid and liquid：Material plate-frame filtering after by enzymolysis, obtains filtered fluid, and drip washing Production With Residue of Enzymatic Hydrolysis 3 times, makes the overwhelming majority
Sugar be dissolved out, obtain leacheate, after leacheate is mixed with filtered fluid, obtain enzymolysis liquid；The now grape in enzymolysis liquid
Sugared purity is 1.9%, and it is 97.1% that the xylan in raw material is converted into the conversion ratio of wood sugar；
4）Concentration：Enzymolysis liquid is concentrated into dry matter content 45% with evaporimeter, concentrate is obtained；
5）Pre- decolouring：The activated carbon that dry matter content adds 1% is pressed in concentrate, is incubated 40min, is filtrated to get decolouring at 75 DEG C
Liquid；
6）Chromatographic isolation is refined：Using three-phase chromatographic separation technology, using Hydrogen separation resin, by destainer be separated into miscellaneous liquid,
Xylose, three components of Arabic liquid glucose；
7）The refined and crystallization of wood sugar：The Xylose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove residual impurity ion,
Wood sugar refined liquid is obtained, concentrated, crystallization, centrifugation obtain xylose crystals；
8）The refined and crystallization of arabinose：The Arabic liquid glucose that chromatographic isolation is obtained sun the moon ion-exchange resins excessively, remove remaining
Foreign ion, obtains arabinose refined liquid, and concentrated, crystallization, centrifugation obtain arabinose crystal.
By specific embodiment above, the those skilled in the art can readily realize the present invention.But should
Work as understanding, the present invention is not limited to above-mentioned several specific embodiments.On the basis of disclosed embodiment, the technology
The technical staff in field can be combined different technical characteristics, so as to realize different technical schemes.
Claims (6)
1. a kind of improved clean manufacturing xylose process, it is characterised in that the xylose production process step is as follows：
1）Pretreatment of raw material：Steam explosion equipment is warming up to 120 DEG C -160 DEG C in advance, agriculture and forestry organic waste material is put into steam explosion equipment then
In, agriculture and forestry organic waste material holdup time in steam explosion equipment is 5min-60min, and 120 DEG C -160 DEG C of steam explosion temperature, every 2s spurt one
Secondary material using mechanical steam recompression device by the Steam Recovery that isolates, and is circulated and is passed through steam explosion to cyclone separator
Equipment steam inlet, through steam explosion after agriculture and forestry organic waste material import enzymatic vessel；
2）Enzymolysis：With the material dry matter content in pure water regulation enzymatic vessel to mass percent 10%-30%, and pH value is adjusted to 3.0-
5.7,40 DEG C -57 DEG C of control system temperature, by 1 ‰ -5 ‰ addition enzyme systems of raw material amount of dry matter, is incubated 10-30h；
3）Separation of solid and liquid：Material plate-frame filtering after by enzymolysis, obtains filtered fluid, and drip washing Production With Residue of Enzymatic Hydrolysis 2-3 time, obtains drip washing
Liquid, obtains enzymolysis liquid with filtered fluid after leacheate is mixed；
4）Concentration：Enzymolysis liquid is concentrated to dryness amount of substance content 30%-50%, concentrate is obtained；
5）Pre- decolouring：The activated carbon that amount of dry matter content adds 1%-2% is pressed in concentrate, at 60-80 DEG C is incubated 30-60min,
It is filtrated to get destainer；
6）Chromatographic isolation is refined：Using three-phase chromatographic separation technology, destainer is separated into by miscellaneous liquid, wood by chromatographic isolation resin
Liquid glucose, three components of Arabic liquid glucose；
7）The refined and crystallization of wood sugar：The Xylose that chromatographic isolation is obtained is crossed cation and anion exchange resin, residual impurity is removed
Ion, obtains wood sugar refined liquid, and concentrated, crystallization, centrifugation obtain xylose crystals；
8）The refined and crystallization of arabinose：The Arabic liquid glucose that chromatographic isolation is obtained is crossed cation and anion exchange resin, is removed
Residual impurity ion, obtains arabinose refined liquid, and concentrated, crystallization, centrifugation obtain arabinose crystal.
2. a kind of improved clean manufacturing xylose process according to claim 1, it is characterised in that described agricultural are discarded
Thing is corncob, bagasse, the one kind in birch-bark.
3. a kind of improved clean manufacturing xylose process according to claim 1, it is characterised in that described step 2）In
Enzyme system by β-Isosorbide-5-Nitrae-endo-xylanase, xylobiase, α-L- furan type arabinosidases, phlorose aldehyde neuraminidase,
Phenolic aldehyde esterase is constituted, and the weight of each constituent is as follows：β-Isosorbide-5-Nitrae-endo-xylanase 1-2 parts, xylobiase
0.5-1 parts, α-L- furan type arabinosidase 0.5-1 parts, phlorose aldehyde neuraminidase 0.5-1 parts, phenolic aldehyde esterase 0.3-0.5
Part.
4. a kind of improved clean manufacturing xylose process according to claim 1, it is characterised in that described chromatographic isolation
Resin is the one kind in sodium form, calcium type and Hydrogen chromatographic isolation resin.
5. a kind of improved clean manufacturing xylose process according to claim 1, it is characterised in that described step 1）In
Before agriculture and forestry organic waste material is put in steam explosion equipment, need continuously to put in steam explosion equipment after water is cleaned or discard agricultural
Thing is put in steam explosion equipment after being put into steam explosion equipment feed well and being soaked with dilute sulfuric acid.
6. a kind of improved clean manufacturing xylose process according to claim 5, it is characterised in that described dilute sulfuric acid
Mass percent concentration is 0.1%-0.5%.
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| CN110042177A (en) * | 2019-05-08 | 2019-07-23 | 河北曌玉科技有限公司 | A kind of hydrolysis of hemicellulose prepares the method and system of xylose |
| CN110468169A (en) * | 2019-09-04 | 2019-11-19 | 吉林省农业科学院 | A kind of method of corncob production L-arabinose |
| CN112210575A (en) * | 2020-11-05 | 2021-01-12 | 浙江科技学院 | Process for preparing xylose by using tea leaves |
| CN112915647A (en) * | 2021-01-26 | 2021-06-08 | 河北易高生物能源有限公司 | Method for recycling steam of blowing boiler |
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| CN112210575A (en) * | 2020-11-05 | 2021-01-12 | 浙江科技学院 | Process for preparing xylose by using tea leaves |
| CN112915647A (en) * | 2021-01-26 | 2021-06-08 | 河北易高生物能源有限公司 | Method for recycling steam of blowing boiler |
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Application publication date: 20170315 |