CN1054130C - Process for recovering xylose from mother solution after xylose crystilization - Google Patents
Process for recovering xylose from mother solution after xylose crystilization Download PDFInfo
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- CN1054130C CN1054130C CN97106079A CN97106079A CN1054130C CN 1054130 C CN1054130 C CN 1054130C CN 97106079 A CN97106079 A CN 97106079A CN 97106079 A CN97106079 A CN 97106079A CN 1054130 C CN1054130 C CN 1054130C
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- xylose
- mother liquor
- wood sugar
- alcohol
- dehydration
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Abstract
The present invention provides a process for recovering xylose from mother solution after xylose crystallization, which comprises the steps that the saturated xylose mother solution containing 15 to 40 percent of water is dehydrated in a low-temperature vacuum state in the methods of vacuum forming, air bubble forming and cyclic magnetization for preparing the xylose mother solution containing about 5 percent of the water; then, a diluting agent of alcohol is added in the mother solution and is stirred uniformly for growing the crystals by standing; finally, the crystals of the xylose are separated from the diluting agent of the alcohol by vacuum filtration and drying, and the crystals of the xylose with the content of 96 to 99 percent are obtained; the diluting agent of the alcohol is recovered for repeated use. Compared with the prior art, the process for recovering the xylose from the mother solution after the xylose crystallization has the characteristics of reasonable design, low investment for equipment, simple process, easy operation, high yield, obvious economic benefit, etc., so the present invention has favorable popularization value and favorable use value.
Description
The present invention relates to a kind of xylose production technical field, specifically a kind of wood sugar technology that behind xylose crystalline, reclaims the mother liquor.
Wood sugar is an important chemical material, is widely used in the industrial production of food, medicine.In foodstuffs industry, can be directly as the sweeting agent of food, in medicine industry, wood sugar can further be processed into Xylitol, the sugariness of Xylitol and thermal value and sucrose are close, and being absorbed by the body does not need Regular Insulin to promote, just can enter cell tissue and carry out normal metabolic, cut and to promote the pancreas excreting insulin, therefore very suitable diabetes patient.In addition, it has the effect that suppresses the upper and lower teeth not meeting properly tooth bacteria live, as the raw material of producing anti-the upper and lower teeth not meeting properly tooth food chewing gum, is that the optimum food of place of sucrose and don't the upper and lower teeth not meeting properly tooth is licked the flavor agent with it.
At present, being in great demand of world's wood sugar, China is maximum in the world xylose production state and export State, and annual all have a large amount of wood sugars to export to countries in the world, and big-and-middle-sized xylose production producer has family more than 80 approximately.In existing xylose production process, the mother liquor behind the xylose crystalline is a byproduct, and one ton of wood sugar of every production is paid the xylose mother liquid that produces the 1-1.5 ton, and xylose mother liquid is sold to foodstuff production producer mainly as food dye.The wood sugar that in xylose mother liquid, contains 30-60%, other compositions are assorted sugar such as water, pectinose, sorbose, seminose, form the heavy-gravity xylose mother liquid, use simple dewatering process to make the xylose mother liquid dehydration, can only make the viscosity increase of xylose mother liquid and the further crystallization of wood sugar is separated out.Some benefit preferably the closed test result that provides of wood sugar factory point out " can in xylose mother liquid, add active carbon purifying and remove impurity; reduce color and luster; put into vacuum pan then and concentrate; can be again xylose crystalline, just rearing crystal time is long, about more than 1000 hours; that gained crystal grain is fine; industrial can't Separation and Recovery, therefore make wood sugar recrystallization from xylose mother liquid reclaim wood sugar can't to be used for suitability for industrialized production by concentrating ", " the recovery xylose crystalline is impossible from xylose mother liquid ".With regard to present xylose production technical field, also do not have sophisticated and can be used for the pertinent literature report of industrial " reclaiming xylose crystalline " from xylose mother liquid.
The purpose of this invention is to provide and a kind ofly can be used for industrially on a large scale, have high yield, less energy-consumption, the technology simple possible behind xylose crystalline, reclaim wood sugar technology the mother liquor.
The objective of the invention is to realize in the following manner, in order to reduce moisture in the xylose mother liquid, adopt dry air bubbling and vacuum dewatering technique that the water content in the xylose mother liquid is reduced to about 5%, in order to reduce wood sugar and other pectinoses, sorbose, assorted sugar such as seminose mixes the viscosity that forms the heavy-gravity xylose mother liquid, making the wood sugar crystallite aggregate into oarse-grained wood sugar crystal separates out from mother liquor, xylose mother liquid after adopting the high strength magnetizing apparatus to dehydration magnetizes, make the wood sugar molecule in the mother liquor produce polarization, improve the intermolecular polar attraction power of wood sugar, thereby can quicken crystalline growth formation macrobead xylose crystalline, add the xylose mother liquid viscosity reduction after the alcohol dilution agent makes dehydration then, wood sugar crystallization from xylose mother liquid is separated out.The recyclable xylose crystalline that accounts for xylose mother liquid 20-30% after separation and drying, that is to say to increase wood sugar yield 20-30% on the basis of existing xylose production process, and the xylose mother liquid after the separation still can be made food color and use.Calculate as turnout, be equivalent to the turnout of newly-built 20 wood sugar factories, thereby economic benefit is considerable by present 80 wood sugar factories.
The wood sugar technology that behind xylose crystalline, reclaims the mother liquor of the present invention, the saturated mother liquor of wood sugar that will contain 15-40% moisture is under the vacuum and low temperature state, adopting vacuum tightness is the 640-740mmHg post, air bubbling under 30-50 ℃ of temperature, make the xylose mother liquid dehydration in 0.5-3.0 ten thousand Gauss's cyclic magnetizations, make the xylose mother liquid that contains moisture about 5%, through leaving standstill growing the grain, volumetric mixture ratio in dehydration back xylose mother liquid and alcohol dilution agent is 1 then: it is even that the ratio of 1-2 adds the alcohol dilution dilution agent, after vacuum filtration, drying makes the wood sugar crystal separate with the alcohol dilution agent, getting content is the wood sugar crystal of 96-99%, and the alcohol dilution agent is reclaimed and reused.
The employed vacuum tightness of vacuum hydro-extraction is the 700mmHg post.
The dehydration temperaturre of xylose mother liquid is controlled at 40 ℃ during the dehydration of air bubbling.
When xylose mother liquid dewater to the mother liquor water content 10% the time, the limit vacuumizes the bubbling dehydration, the limit starts surge pump makes mother liquor cyclic magnetization in the pipeline magnetizing apparatus, and until making the mother liquor water content reduce to 5%, the employed optimum magnetic field intensity of pipeline magnetizing apparatus is 2.0 ten thousand Gausses.
The mother liquor water content was reduced to 5% o'clock, made mother liquor cool the temperature to 20-25 ℃ with water coolant, left standstill growing the grain and crystal was grown up in 12 hours.
The employed thinner of dilution mother liquor can be methyl alcohol, ethanol, Virahol or two or more alcohol mixtures, and concentration of ethanol is 95%.
The optimal volume ratio of mixture of dehydration back xylose mother liquid and alcohol dilution agent is 1: 1.5.
Embodiment:
Concrete enforcement of reclaiming wood sugar technology behind xylose crystalline the mother liquor of the present invention is as follows;
Processed: the saturated mother liquor of wood sugar that will contain 15-40% moisture is squeezed in the retort of belt stirrer and strap clamp shell type with volume pump, starting vacuum pump makes jar interior vacuum tightness reach the 740mmHg post, feed dry air then by bubbling under the liquid level, in the retort chuck, feed hot water the mother liquor temperature is remained on about 40 ℃.
Cyclic magnetization is handled: when the mother liquor water content is reduced to 10% left and right sides, starting surge pump handles mother liquor cyclic magnetization between retort and pipeline magnetizing apparatus, water content is reduced to about 5% in mother liquor, stop magnetization and dehydration, feed water coolant and make the mother liquor temperature reduce to 20 ℃ in chuck, growing the grain is 12 hours under this temperature.
Separate and carrying out precipitation treatment: 95% the ethanol that in retort, adds 1.5 times of suitable xylose mother liquid volumes, starting agitator stirs, send the vacuum filter vacuum filtration with surge pump with art sugar mother liquor and alcohol dilution agent, and with small amount of ethanol thinner washing xylose crystalline 1-2 time, drain solvent, directly send 85 ℃ of cylinder drying machine internal heating with xylose crystalline, will be clean under the vacuum of 700mmHg post attached to the solvent removal on xylose crystalline surface, just can reclaim the xylose crystalline that content is 96-99%.Yield is at 20-30%.
The recovery of alcohol dilution agent: send into the xylose mother liquid that leaches and the mixed solution of alcohol dilution agent in the retort of belt stirrer with surge pump, reclaim the alcohol dilution agent under 700-740mmHg post vacuum tightness state, the alcohol dilution agent after the recovery can continue to recycle.The tail gas that vacuum filtration and xylose crystalline vacuum-drying are discharged is refrigerated to-15--20 ℃ by condenser, and alcohol dilution agent condensation is reclaimed, and the rate of recovery of alcohol dilution agent is more than 96%.
The wood sugar technology that reclaims the mother liquor behind xylose crystalline of the present invention, the wood sugar content of recovery is at 96-99%, (detecting with the liquid spectrometry) the recyclable xylose crystalline 150-200 of xylose mother liquid per ton kilogram.Production cost with the xylose crystalline that this method obtained is about the 1/2-1/3. of existing xylose production cost because the raising of xylose production total recovery, therefore can reduce existing more than 20% of xylose production cost, the rate of recovery of the employed alcohol dilution agent of this technology can reach more than 96%, xylose mother liquid after the recovery is behind desolventizing, contain the wood sugar and the assorted sugar of small part, still can make the raw material that food dye or other medication chemistries are produced.
The facility investment of reclaiming wood sugar technology behind xylose crystalline the mother liquor is about 1/4 of newly-built equal scale wood sugar factory.
Below be to be sample, make to reclaim the testing data contrast situation of xylose crystalline with technology of the present invention with the saturated mother liquor of wood sugar behind three wood sugar factory xylose crystallines:
1, from * * * to get water content be 100 kilograms in 19.5% the saturated mother liquor of wood sugar in wood sugar factory: the dehydration magnetization is handled the crystalline condition wood sugar and must be measured wood sugar and contain % ℃ of mmHg liquid of amount temperature vacuum tightness Kg spectrometry 50-70 〉=700 and handle no crystallization
The no crystallization 30-40 〉=fast grain of 700 processing crystallizations that is untreated is big by 18.3 98.7
The slow grain of the crystallization of being untreated is little by 17.0 97.6
2, from * * to get water content be 100 kilograms in 40.0% the saturated mother liquor of wood sugar in wood sugar factory: the dehydration magnetization is handled the crystalline condition wood sugar and must be measured wood sugar and contain % ℃ of mmHg liquid of amount temperature vacuum tightness Kg spectrometry 50-70 〉=700 and handle no crystallization
The no crystallization 30-40 〉=fast grain of 700 processing crystallizations that is untreated is big by 15.6 98.9
The slow grain of the crystallization of being untreated is little by 15.0 98.3
3, from * * to get water content be 100 kilograms in 15% the saturated mother liquor of wood sugar in wood sugar factory: the dehydration magnetization is handled the crystalline condition wood sugar and must be measured wood sugar and contain % ℃ of mmHg liquid of amount temperature vacuum tightness Kg spectrometry 50-70 〉=700 and handle no crystallization
The no crystallization 30-40 〉=fast grain of 700 processing crystallizations that is untreated is big by 20.0 99
The slow grain of the crystallization of being untreated is little by 18.7 98.1
In above three embodiment, used methyl alcohol, ethanol, Virahol or two kinds of alcohol mixtures to make thinner respectively, the gained result is roughly the same.
The wood sugar technology that reclaims the mother liquor behind xylose crystalline of the present invention is compared with prior art, have reasonable in design, facility investment is little, technology is simple, easy to implement, characteristics such as yield is high, remarkable in economical benefits, can supporting use in existing or newly-built wood sugar factory production technique, wood sugar output is had a net increase of produce 20-30%, the xylose mother liquid after the separation still can be made food color and use.As calculating by existing 80 the wood sugar factory turnout of present China, use technology of the present invention after, be equivalent to the turnout of newly-built 20 equal scale wood sugar factories, economic benefit is considerable.Therefore has well extensive popularizing value.
Claims (7)
1. behind xylose crystalline, reclaim wood sugar technology the mother liquor, it is characterized in that to contain the saturated mother liquor of wood sugar of 15-40% moisture under the vacuum and low temperature state, adopting vacuum tightness is the 640-740mmHg post, air bubbling under 30-50 ℃ of temperature, make the xylose mother liquid dehydration in 0.5-3.0 ten thousand Gauss's cyclic magnetizations, make the xylose mother liquid that contains moisture about 5%, through leaving standstill growing the grain, volumetric mixture ratio in dehydration back xylose mother liquid and alcohol dilution agent is 1 then: it is even that the ratio of 1-2 adds the alcohol dilution dilution agent, after vacuum filtration, drying makes the wood sugar crystal separate with the alcohol dilution agent, getting content is the wood sugar crystal of 96-99%, and the alcohol dilution agent is reclaimed and reused.
2, technology according to claim 1 is characterized in that the employed vacuum tightness of vacuum hydro-extraction is the 700mmHg post.
3, technology according to claim 1, the dehydration temperaturre of xylose mother liquid is controlled at 40 ℃ when it is characterized in that the dehydration of air bubbling.
4, technology according to claim 1, it is characterized in that when xylose mother liquid dewater to the mother liquor water content 10% the time, the limit vacuumizes the bubbling dehydration, the limit starts surge pump makes mother liquor cyclic magnetization in the pipeline magnetizing apparatus, until making the mother liquor water content reduce to 5%, the employed optimum magnetic field intensity of pipeline magnetizing apparatus is 2.0 ten thousand Gausses.
5, technology according to claim 1 is characterized in that the mother liquor water content reduced at 5% o'clock, makes mother liquor cool the temperature to 20-25 ℃ with water coolant, leaves standstill growing the grain and crystal is grown up in 12 hours.
6, technology according to claim 1, it is characterized in that diluting the employed thinner of mother liquor can be methyl alcohol, ethanol, Virahol or two or more alcohol mixtures, concentration of ethanol is 95%.
7, technology according to claim 1, the optimal volume ratio of mixture of xylose mother liquid and alcohol dilution agent is 1: 1.5 after it is characterized in that dewatering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106079A CN1054130C (en) | 1997-09-08 | 1997-09-08 | Process for recovering xylose from mother solution after xylose crystilization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106079A CN1054130C (en) | 1997-09-08 | 1997-09-08 | Process for recovering xylose from mother solution after xylose crystilization |
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| Publication Number | Publication Date |
|---|---|
| CN1210862A CN1210862A (en) | 1999-03-17 |
| CN1054130C true CN1054130C (en) | 2000-07-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN97106079A Expired - Fee Related CN1054130C (en) | 1997-09-08 | 1997-09-08 | Process for recovering xylose from mother solution after xylose crystilization |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365006C (en) * | 2004-06-24 | 2008-01-30 | 华东理工大学 | Method for reclaiming xylose from hydrolyzed fermented biomass waste liquid |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102580611B (en) * | 2011-12-15 | 2013-11-06 | 重庆大学 | Method for processing xylose mother solutions |
| CN103172604B (en) * | 2011-12-22 | 2015-06-24 | 北大方正集团有限公司 | Lovastatin purification method combining auxiliary magnetic crystallization |
| CN104892689B (en) * | 2015-06-24 | 2018-03-27 | 济南圣泉集团股份有限公司 | A kind of processing method of xylose mother liquid |
| CN113004346A (en) * | 2021-02-07 | 2021-06-22 | 济南茂腾生物科技有限公司 | Method for preparing xylose by negative pressure coupling normal pressure crystallization |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032940A (en) * | 1988-11-12 | 1989-05-17 | 福建省漳州糖厂 | The preparation method of crystalline xylose |
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1997
- 1997-09-08 CN CN97106079A patent/CN1054130C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032940A (en) * | 1988-11-12 | 1989-05-17 | 福建省漳州糖厂 | The preparation method of crystalline xylose |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100365006C (en) * | 2004-06-24 | 2008-01-30 | 华东理工大学 | Method for reclaiming xylose from hydrolyzed fermented biomass waste liquid |
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| CN1210862A (en) | 1999-03-17 |
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