CN104892689B - A kind of processing method of xylose mother liquid - Google Patents
A kind of processing method of xylose mother liquid Download PDFInfo
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- CN104892689B CN104892689B CN201510354543.8A CN201510354543A CN104892689B CN 104892689 B CN104892689 B CN 104892689B CN 201510354543 A CN201510354543 A CN 201510354543A CN 104892689 B CN104892689 B CN 104892689B
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- sugar
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- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 281
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 145
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000007788 liquid Substances 0.000 title claims abstract description 117
- 238000003672 processing method Methods 0.000 title claims abstract description 25
- 235000000346 sugar Nutrition 0.000 claims abstract description 76
- 239000013078 crystal Substances 0.000 claims abstract description 21
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 238000010792 warming Methods 0.000 claims abstract description 18
- 238000001728 nano-filtration Methods 0.000 claims description 19
- 238000000108 ultra-filtration Methods 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011549 crystallization solution Substances 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 claims description 4
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 claims description 4
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 235000010358 acesulfame potassium Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000012360 testing method Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 30
- 239000012528 membrane Substances 0.000 description 16
- 150000003742 xyloses Chemical class 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 239000012452 mother liquor Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 229920006393 polyether sulfone Polymers 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 150000008163 sugars Chemical class 0.000 description 3
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- MIDXCONKKJTLDX-UHFFFAOYSA-N 3,5-dimethylcyclopentane-1,2-dione Chemical compound CC1CC(C)C(=O)C1=O MIDXCONKKJTLDX-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-HWQSCIPKSA-N L-arabinopyranose Chemical compound O[C@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-HWQSCIPKSA-N 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000013736 caramel Nutrition 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention provides a kind of processing method of xylose mother liquid, comprise the following steps：A it is 80~92% that it is dense that xylose mother liquid) is concentrated into total reducing sugar, the xylose mother liquid concentrated；B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, then starts to cool, 60~70 DEG C of addition crystal seeds is down to, when temperature is down to 20~25 DEG C, is crystallized, obtain crystallized product and the first miscellaneous sugar liquid；C) by the step B) obtained crystallized product recrystallized, obtain xylose and miscellaneous sugar liquid.The present invention is by controlling first subcrystalline technique so that xylose mother liquid can be succinct with direct crystallization, technological process, it is workable, and the yield of xylose is higher, test result indicates that, the xylose purity of the processing method of the present invention is used as 99%, yield is 40~50%.
Description
Technical field
The invention belongs to technical field of biochemical industry, more particularly to a kind of processing method of xylose mother liquid.
Background technology
Xylose mother liquid is obtained byproduct after producing crystal xylose as raw material using corncob, Main Ingredients and Appearance be xylose, Ah
Uncle's sugar, glucose and galactolipin etc. are drawn, dense total reducing sugar is 65~70% or so.Wherein xylose and L-arabinose are azymic sugar,
The 70% of total reducing sugar is accounted for, both sugared values are very high；Glucose, galactolipin etc. are fermentable sugars, account for the 26% of total reducing sugar, both
Sugar value is relatively low；Other saccharic compositions also have the miscellaneous sugars such as mannose, rhamnose, account for the 4% of total reducing sugar.Xylose mother liquid is because miscellaneous sugar content
Height, xylose purity are low, it is difficult to purify the xylose crystalline in mother liquor.The large-scale application of xylose mother liquid is concentrated mainly on institute at present
In integrated application containing monose, such as caramel colorant is prepared, production fodder yeast etc., these can not make various monose in mother liquor
Value fully played.
It is certain by being added into the xylose mother liquid for being difficult to crystallize in the A of Publication No. CN 102964393 Chinese patent
The xylose of amount improves the xylose purity in Xylose from liquid (xylose mother liquid is 1 with the weight ratio from friendship liquid: (1~10)) is handed over,
Then the pigment in mixed sugar liquid and polysaccharide are removed after UF membrane together with filter membrane, carries out obtaining xylose from crystallization after friendship.
The above method can crystallize from xylose mother liquid and obtain xylose, but this method has a complex process, and cost is higher etc.
Problem, it is difficult to industrial applications.
The content of the invention
It is an object of the invention to provide a kind of processing method of xylose mother liquid, the technique of processing method provided by the invention
Simply, direct crystallization can obtain xylose, and yield is higher, be 40~50%.
The present invention provides a kind of processing method of xylose mother liquid, comprises the following steps：
A it is 80~92% that it is dense that xylose mother liquid) is concentrated into total reducing sugar, the xylose mother liquid concentrated；
B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, then starts to cool, 60~70 DEG C is down to and adds crystalline substance
Kind, when temperature is down to 20~25 DEG C, crystallized, obtain crystallized product and the first miscellaneous sugar liquid；
C) by the step B) obtained crystallized product recrystallized, obtain xylose and the second miscellaneous sugar liquid.
Preferably, the step B) after also include：
By the step B) in the first miscellaneous sugar liquid extraction miscellaneous sugar, the miscellaneous sugar include arabinose, glucose, gala
One or more in sugar, mannose and rhamnose.
Preferably, the step A) also include before：
By xylose mother liquid be diluted to total reducing sugar it is dense be 5~30% after, carry out ultrafiltration and nanofiltration successively, obtain the xylose after nanofiltration
Mother liquor.
Preferably, the temperature of the ultrafiltration is 10~50 DEG C；
The pressure of the ultrafiltration is 1~7bar.
Preferably, the temperature of the nanofiltration is 10~50 DEG C；
The pressure of the nanofiltration is 3.5~30bar.
Preferably, the step B) in, when temperature is down to 20~25 DEG C, solvent is added, is crystallized；
The solvent includes the one or more in methanol, ethanol and chilled water；
The quality of the solvent is the 0.1~20% of the xylose mother liquid quality of the concentration.
Preferably, the step B) in cooling speed be 0.3~1 DEG C/h.
Preferably, the step B) in crystal seed quality for the concentration xylose mother liquid quality 0.1~1%.
Preferably, the step B) in crystallized after, in addition to, the mixture after crystallization is squeezed, tied
Brilliant product and the first miscellaneous sugar liquid.
Preferably, the step C) in recrystallization specifically include：
The crystallized product is dissolved in water, obtains crystallization solution, the crystallization solution is warming up to 75~80 DEG C, Ran Houkai
Begin to cool, be down to 70~75 DEG C of addition crystal seeds, temperature is crystallized when being down to 25~30 DEG C, obtains xylose and the second miscellaneous sugar liquid.
The invention provides a kind of processing method of xylose mother liquid, comprise the following steps：A) xylose mother liquid is concentrated into always
Dense sugar is 80~92%, the xylose mother liquid concentrated；B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, Ran Houkai
Begin to cool, be down to 60~70 DEG C of addition crystal seeds, temperature adds solvent when being down to 20~25 DEG C, crystallized, and obtains crystallized product
With the first miscellaneous sugar liquid；C) by the step B) obtained crystallized product recrystallized, obtain xylose and the second miscellaneous sugar liquid.This hair
It is bright to pass through first subcrystalline technique of control so that xylose mother liquid can be with direct crystallization, and technological process is succinct, workable,
And the yield of xylose is higher, test result indicates that, the xylose purity of processing method of the present invention is used as 99%, yield 40
~50%.
Further, the present invention is crystallized again after also xylose mother liquid can first being carried out into ultrafiltration and nanofiltration, and the step can incite somebody to action
Pigment and polysaccharide in xylose mother liquid remove, further the yield of raising xylose to 65~80%, purity 99%.
In addition, processing method provided by the invention is green, the discharge of pollutant is less.
Embodiment
The invention provides a kind of processing method of xylose mother liquid, comprise the following steps：
A it is 80~92% that it is dense that xylose mother liquid) is concentrated into total reducing sugar, the xylose mother liquid concentrated；
B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, then starts to cool, 60~70 DEG C is down to and adds crystalline substance
Kind, temperature adds solvent when being down to 20~25 DEG C, crystallized, and obtains crystallized product and the first miscellaneous sugar liquid；
C) by the step B) obtained crystallized product recrystallized, obtain xylose and the second miscellaneous sugar liquid.
Processing method technique provided by the invention is simple, workable, and xylose yield is 40~50%, and purity is
99%.
In order to further improve the yield of xylose, the present invention is first dilute by xylose mother liquid preferably before xylose mother liquid is concentrated
It is 5~30% to release to solid content, then carries out ultrafiltration and nanofiltration successively, obtains the xylose mother liquid after nanofiltration.The present invention preferably will
Xylose mother liquid mixes with water, and it is 5~30% to be diluted to solid content, is more preferably diluted to 10~20%, then carries out ultrafiltration successively
And nanofiltration, obtain the xylose mother liquid after nanofiltration.The present invention does not have special limitation to the source of described xylose mother liquid, preferably adopts
With caused xylose mother liquid in corncob process, in general, the mass concentration of xylose mother liquid is 65~70%.
In the present invention, the temperature of the ultrafiltration is preferably 10~50 DEG C, more preferably 20~45 DEG C, most preferably 30~
40℃；The pressure of the ultrafiltration is preferably 1~7bar, more preferably 2~6bar, most preferably 3~5bar；The present invention preferably adopts
Ultrafiltration is carried out with milipore filter, the aperture of the milipore filter is preferably 5000~100000 dalton, more preferably 10000~
90000 dalton, most preferably 20000~80000 dalton；The milipore filter is preferably hollow-fibre membrane, tubular membrane, ceramics
One or more in film and poly (ether sulfone) film.
In the present invention, the temperature of the nanofiltration is preferably 10~50 DEG C, more preferably 20~45 DEG C, most preferably 30~
40℃；The pressure of the ultrafiltration is preferably 3.5~30bar, more preferably 10~25bar, most preferably 15~20bar；This hair
Bright preferably to carry out nanofiltration using NF membrane, the aperture of the NF membrane is preferably 100~2500 dalton, more preferably 500~
2000 dalton, most preferably 800~1500 dalton；The NF membrane is preferably poly (ether sulfone) film, sulfonated polyether sulfone film, polyester
One or more in film, PS membrane, aromatic polyamides film, polyvinyl alcohol film and poly- piperazine film..
It is 80~92% that xylose mother liquid after nanofiltration preferably it is dense, which to be concentrated into total reducing sugar, by the present invention, i.e. in the xylose mother liquid
Sugared total mass concentration of contained all kinds.The xylose mother liquid concentrated, present invention preferably employs triple effect and single-action
Evaporator concentrates the xylose mother liquid after the nanofiltration.
After the xylose mother liquid concentrated, the xylose mother liquid of concentration is warming up to 70~80 DEG C by the present invention, then starts to drop
Temperature, 60~70 DEG C of addition crystal seeds are down to, when temperature is down to 20~25 DEG C, is crystallized, obtains crystallized product and the first miscellaneous sugar liquid；
The xylose of concentration is preferably warming up to 70~80 DEG C by the present invention, then starts to cool, and is down to 60~70 DEG C of addition crystal seeds, temperature drop
Solvent is added during to 20~25 DEG C, is crystallized, after terminating, the mixture after crystallization is squeezed, obtains crystallization production
Thing and the first miscellaneous sugar liquid；The xylose of concentration is more preferably warming up to 73~78 DEG C by the present invention, is then started to cool, is down to 63~68
DEG C add crystal seed, temperature adds solvent when being down to 22~24 DEG C, crystallized, and after terminating, the mixture after crystallization is entered
Row squeezing, obtains crystallized product and the first miscellaneous sugar liquid.
The xylose mother liquid of the concentration is preferably down to 20~25 DEG C by the present invention with identical cooling rate from 70~80 DEG C,
The rate of temperature fall is preferably 0.3~1 DEG C/h, more preferably 0.5~0.8 DEG C/h；The crystal seed is preferably after crushing
Xylose, the quality of the crystal seed is preferably the 0.1~1% of massecuite quality, more preferably 0.2~0.8%, most preferably 0.4
~0.6%；The solvent preferably includes the one or more in methanol, ethanol and chilled water, and the quality of the solvent is preferably
0.1~20% of xylose mother liquid quality after the concentration, more preferably 1~15%, most preferably 5~10%.
After completing the crystallization, the mixture that crystallization obtains preferably is squeezed or centrifuged by the present invention, to extract knot
Brilliant product, remaining first miscellaneous sugar liquid is removed, it is special that the present invention does not have to the method for the squeezing and press apparatus used
Limitation, e.g., can use plate and frame squeezer；The method of the centrifugation is the centrifugal method that those skilled in the art commonly use.
In the present invention, the first miscellaneous sugar liquid can be used for extracting miscellaneous sugar, and the miscellaneous sugar preferably includes arabinose, grape
One or more in sugar, galactolipin, mannose and rhamnose, the extracting method of the miscellaneous sugar is conventional method.
After obtaining crystallized product, the present invention is recrystallized the crystallized product, obtains xylose and the second miscellaneous sugar liquid, this
The crystallized product is preferably dissolved in water by invention, obtains crystallization solution, the crystallization solution is warming up into 75~80 DEG C, Ran Houkai
Begin to cool, rate of temperature fall is preferably 0.3~1 DEG C/h, more preferably 0.5~0.8 DEG C/h, is down to 70~75 DEG C and adds crystalline substance
Kind, the crystal seed is preferably the xylose crushed, is crystallized, obtained when temperature rate being cooled the temperature into 25~30 DEG C with identical
Xylose and the second miscellaneous sugar liquid.
In the present invention, the second miscellaneous sugar liquid is similar with the composition of xylose mother liquid, the second miscellaneous sugar liquid that will can be obtained
Mix with original xylose mother liquid, then using the processing method of above-mentioned xylose mother liquid, obtained mixing mother liquor is extracted
Xylose and other miscellaneous sugars, so can not only improve xylose yield, additionally it is possible to and it is cost-effective, improve industrialization efficiency.
The invention provides a kind of processing method of xylose mother liquid, comprise the following steps：A) xylose mother liquid is concentrated into always
Dense sugar is 80~92%, the xylose mother liquid concentrated；B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, Ran Houkai
Begin cooling, be down to 60~70 DEG C of addition crystal seeds, when temperature is down to 20~25 DEG C, crystallized, obtain crystallized product and first miscellaneous
Liquid glucose；C) by the step B) obtained crystallized product recrystallized, obtain xylose and the second miscellaneous sugar liquid.The present invention passes through control
Make first subcrystalline technique so that xylose mother liquid can be with direct crystallization, and technological process is succinct, workable, and xylose
Yield it is higher, test result indicates that, use the present invention processing method xylose purity for 99%, yield be 40~50%.
Further, the present invention is crystallized again after also xylose mother liquid can first being carried out into ultrafiltration and nanofiltration, and the step can incite somebody to action
Pigment and polysaccharide in xylose mother liquid remove, further the yield of raising xylose to 65~80%, purity 99%.
In addition, processing method provided by the invention is green, the discharge of pollutant is less.
In order to further illustrate the present invention, with reference to embodiments to a kind of processing side of xylose mother liquid provided by the invention
Method is described in detail, but can not be understood as limiting the scope of the present invention.
Embodiment 1
By 1000g xylose mother liquids (Xylose Content 31.5%, other miscellaneous sugar contents 24% in xylose mother liquid), single effect evaporation is used
After device is concentrated into sugar dense 80%, 70 DEG C are warming up to, then starts to cool, reduced by 0.3 DEG C per hour, added when being down to 60 DEG C
0.83g crystal seeds, treat that temperature is down to 20 DEG C and crystallized, squeezed after crystallization with plate and frame squeezer, obtained solid
For crystallized product, liquid is miscellaneous sugar liquid, and the xylose purity in crystallized product can obtain after 75%, dissolving by crystallizing again
154g finished product xyloses, the purity of xylose is 99%, and xylose yield is 48.4%.
Embodiment 2
By 1000g xylose mother liquids (Xylose Content 29.8%, other miscellaneous sugar contents 25.6% in xylose mother liquid), steamed with single-action
After hair device is concentrated into sugar dense 85%, 80 DEG C are warming up to, then starts to cool, reduced by 1 DEG C per hour, added when being down to 70 DEG C
4.12g crystal seed, treat that temperature is down to 25 DEG C of addition 165g methanol, crystallized, centrifuged after crystallization with centrifuge, obtained
The solid arrived is crystallized product, and liquid is miscellaneous sugar liquid, and the xylose purity in crystallized product is after 70%, dissolving by crystallizing again
135g finished product xyloses can be obtained, the purity of xylose is 99%, and xylose yield is 45.3%.
Embodiment 3
By 1000g xylose mother liquids (Xylose Content 27.4%, other miscellaneous sugar contents 27.6% in xylose mother liquid), steamed with single-action
After hair device is concentrated into sugar dense 92%, 75 DEG C are warming up to, then starts to cool, reduced by 1 DEG C per hour, added when being down to 65 DEG C
7.52g crystal seed, treat that temperature is down to 25 DEG C of addition 42.5g chilled waters, crystallized, entered after crystallization with plate and frame squeezer
Row squeezing, obtained solid is crystallized product, and liquid is miscellaneous sugar liquid, and the xylose purity in crystallized product passes through after 70%, dissolving
117g finished product xyloses can be obtained by crossing crystallization again, and the purity of xylose is 99%, and xylose yield is 42.7%.
Embodiment 4
It is first dilute with water by 10kg xylose mother liquids (Xylose Content 30.7%, other miscellaneous sugar contents 25.2% in xylose mother liquid)
Release to total reducing sugar dense 5%, then cross milipore filter (hollow-fibre membrane) under 10 DEG C, 1bar pressure, obtained light phase again 10 DEG C,
5bar pressure descended NF membrane (the DK films of GE companies), after the light phase of sodium filter membrane is concentrated into sugar dense 80%, was warming up to 75 DEG C, so
After start to cool, reduce by 1 DEG C per hour, 8.75g crystal seed added when being down to 65 DEG C, treat temperature to be down to 25 DEG C that to add 82.35g cold
Freeze water, crystallized, crystallized product and miscellaneous sugar liquid are obtained after centrifugation, by tying again after then obtained crystallized product is dissolved
Crystalline substance, 2333g finished product xyloses are can obtain after centrifugation, the purity of xylose is 99%, and xylose yield is 76%.
Embodiment 5
10kg xylose mother liquids (Xylose Content 28.6%, other miscellaneous sugar contents 26.3% in xylose mother liquid), are first diluted with water
To total reducing sugar dense 30%, milipore filter (tubular membrane) then is crossed under 40 DEG C, 7bar pressure, obtained light phase is again in 50 DEG C, 30bar
Pressure descended NF membrane (Tao Shi NF-200), after the light phase of sodium filter membrane is concentrated into sugar dense 92%, was warming up to 80 DEG C, Ran Houkai
Begin to cool, reduce by 0.5 DEG C per hour, 15.6g crystal seed is added when being down to 65 DEG C, treat that temperature is down to 25 DEG C and adds 102.3g freezings
Water, crystallized, squeezed after crystallization with plate and frame squeezer, 2010g finished product xyloses are can obtain after squeezing, xylose
Purity is 99%, and xylose yield is 70.3%.
Embodiment 6
It is first dilute with water by 10kg xylose mother liquids (Xylose Content 26.8%, other miscellaneous sugar contents 28.3% in xylose mother liquid)
Release to sugar dense 20%, then cross milipore filter under 30 DEG C, 5bar pressure, the obtained light phase mistake under 40 DEG C, 25bar pressure again
NF membrane, after the light phase of sodium filter membrane is concentrated into sugar dense 90%, 70 DEG C are warming up to, then starts to cool, reduces by 0.6 per hour
DEG C, 36.5g crystal seed is added when being down to 60 DEG C, treats that temperature is down to 20 DEG C of addition 152.4g chilled waters, is crystallized, crystallization finishes
After centrifuged, can obtain 1796g finished product xyloses, the purity of xylose is 99%, and xylose yield is 67%.
As can be seen from the above embodiments, not only technique is simple for xylose mother liquid processing method provided by the invention, is easy to grasp
Make, and obtained xylose purity is high, high income.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of processing method of xylose mother liquid, comprises the following steps：
A it is 80~92% that the xylose mother liquid after nanofiltration) is concentrated into total sugar concentration, the xylose mother liquid concentrated；
B the xylose mother liquid of the concentration) is warming up to 70~80 DEG C, then starts to cool, is down to 60~70 DEG C of addition crystal seeds, temperature
When degree is down to 20~25 DEG C, is crystallized, obtain crystallized product and the first miscellaneous sugar liquid；
C) by the step B) obtained crystallized product recrystallized, obtain xylose and the second miscellaneous sugar liquid；
The step A) also include before：
Xylose mother liquid is diluted to total sugar concentration after 5~30%, to carry out ultrafiltration and nanofiltration successively, obtains the mother of the xylose after nanofiltration
Liquid；
The temperature of the ultrafiltration is 10~50 DEG C；The pressure of the ultrafiltration is 1~7bar；The temperature of the nanofiltration is 10~50
℃；The pressure of the nanofiltration is 3.5~30bar.
2. processing method according to claim 1, it is characterised in that the step B) after also include：
By the step B) in the first miscellaneous sugar liquid extraction miscellaneous sugar, the miscellaneous sugar includes arabinose, glucose, galactolipin, sweet
One or more in dew sugar and rhamnose.
3. according to the processing method described in claim 1~2 any one, it is characterised in that the step B) in, when temperature drops
During to 20~25 DEG C, solvent is added, is crystallized；
The solvent includes the one or more in methanol, ethanol and chilled water；
The quality of the solvent is the 0.1~20% of the xylose mother liquid quality of the concentration.
4. according to the processing method described in claim 1~2 any one, it is characterised in that the step B) in cooling speed
Rate is 0.3~1 DEG C/h.
5. according to the processing method described in claim 1~2 any one, it is characterised in that the step B) in crystal seed matter
Measure 0.1~1% of the xylose mother liquid quality for the concentration.
6. according to the processing method described in claim 1~2 any one, it is characterised in that the step B) in crystallized
Also include afterwards, the mixture after crystallization is squeezed, obtain crystallized product and the first miscellaneous sugar liquid.
7. according to the processing method described in claim 1~2 any one, it is characterised in that the step C) in recrystallization
Specifically include：
The crystallized product is dissolved in water, obtains crystallization solution, the crystallization solution is warming up to 75~80 DEG C, then starts to drop
Temperature, 70~75 DEG C of addition crystal seeds are down to, temperature is crystallized when being down to 25~30 DEG C, obtains xylose and the second miscellaneous sugar liquid.
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| CN107892644A (en) * | 2017-12-08 | 2018-04-10 | 山东福田药业有限公司 | A kind of method that xylitol is reclaimed from more subcrystalline Xylitol mother liquor |
| CN111944486B (en) * | 2019-05-16 | 2023-06-16 | 济南圣泉集团股份有限公司 | Saccharide mixture and preparation method and application thereof |
| CN113025516A (en) * | 2020-12-28 | 2021-06-25 | 浙江华康药业股份有限公司 | Method for preparing xylitol by fermenting xylose secondary mother liquor |
| CN114213215B (en) * | 2021-12-29 | 2023-11-10 | 浙江华康药业股份有限公司 | System and method for co-producing xylitol and caramel pigment by utilizing xylose mother liquor |
| CN116694830B (en) * | 2023-07-19 | 2025-09-19 | 浙江华康药业股份有限公司 | Method for extracting finished xylose from xylose mother liquor |
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