CN101284849A - Process for purifying xylose mother liquor by sequential simulated moving bed - Google Patents
Process for purifying xylose mother liquor by sequential simulated moving bed Download PDFInfo
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- CN101284849A CN101284849A CNA2007100141758A CN200710014175A CN101284849A CN 101284849 A CN101284849 A CN 101284849A CN A2007100141758 A CNA2007100141758 A CN A2007100141758A CN 200710014175 A CN200710014175 A CN 200710014175A CN 101284849 A CN101284849 A CN 101284849A
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Abstract
A method for separating xylose mother liquor by means of a sequential analog moving bed relates to a method for making purified xylose mother liquor. The method mainly comprises the following steps that: (1) sequential analog moving bed separation technology is adopted to separate xylose mother liquor, and water is used as an eluant with the separation temperature of between 30 and 90 DEG C; (2) the xylose mother liquor is allowed to pass through a chromatographic column filled with chromatogram separation resin, so as to ensure that the xylose positioned at the middle part of an outflow curve can be fully separated; (3) a sequential analog moving bed separating device is adopted to separate the xylose mother liquor, and calcium type strongly acidic cationic resin is used as a separating agent. Meanwhile, the invention provides a separating device capable of increasing the purity of the xylose mother liquor, wherein the device is filled inside with chromatogram separation resin; the xylose mother liquor passes through the resin with water acted as mobile phase; thus, xylose can be purified through the technological process of the device. The separating device can separate the xylose mother liquor without removing the glucose composition in the xylose mother liquor; moreover, the separating device has high yield, high purity and easy crystallization, and greatly increases the economic benefit of the xylose mother liquor.
Description
Technical field
The invention belongs to technical field of functional sugar production, relate to the preparation method of wood sugar.
Background technology
Xylose product mainly is to be raw material with agricultural byproducts such as corn cob, bagasse, and the white crystals body through operations such as hydrolysis, purification, evaporation, crystallization, centrifugal, oven dry are made is widely used in the industries such as light industry, food, chemical industry.Because it extracts from plant waste, often contain impurity such as pectinose, glucose and exist, influenced the crystallization of wood sugar and the raising of yield, calculate according to producing, 1 ton of crystalline xylose of every production can produce 1.5 tons of xylose mother liquids, and mother liquid concentration wherein contains wood sugar 50-70% about 60%, glucose 5-15%, pectinose 15-30% is because the existence of these assorted sugar makes xylose mother liquid recrystallize again, can only sell as byproduct, marketable value is very low.Chinese patent 200510040433.0 discloses a kind of method of purifying xylose mother liquor, it at first utilizes the glucose in the yeast saccharomyces cerevisiae removal xylose mother liquid, adopting simulation moving-bed then is that traditional SMB isolation technique is separated xylose mother liquid, and xylose mother liquid is separated into the component that is rich in wood sugar and the component of assorted liquid glucose.Charging and discharging of this kind separate mode and recycle to extinction are carried out continuously, charging and discharging are carried out with synchro cut, flow out part before can only being divided into raw material by the chromatogram elution curve and flow out part with the back, carrying out two portions separates, it is to purify at elution curve forefront or aftermost being easy to target product, but is just not good at the refining effect at middle part to target product.And we find in analysis, there is 4-5 assorted sugar front, wood sugar peak in the chromatographic peak of xylose mother liquid, the back has pectinose to exist, so adopt this kind separate mode, efficient is very low, and in this technology, introduced and adopted yeast saccharomyces cerevisiae to remove the operation of glucose, running cost is significantly increased, be difficult to utilization and extention.
Summary of the invention
The objective of the invention is the method for seeking a kind of better purifying xylose mother liquor, adopt the technology of high efficiency separation,, improve the purity and the yield of product to obtain more purity of xylose product based on simulation moving-bed isolating basis.
The main technical schemes of the inventive method comprises: 1. adopt sequential simulated moving bed isolation technique that xylose mother liquid is separated.2. used resin is commercially available chromatographic separation resin, need not special preparation.3. xylose mother liquid is well separated by the chromatographic column of chromatographic separation resin being housed, making the wood sugar that is positioned at the elution curve middle part, made the xylose solution of higher degree.
Sequential simulated moving bed tripping device of the present invention is that the chromatographic column by the 4-10 root is connected in series, the loop system (referring to accompanying drawing 1) that becomes head and the tail to connect.Import at every root chromatogram column all has charging, two mouths of water inlet, outlet at every root chromatogram column all has three classes to flow out the component outlet, and this three class flows out component to be represented in order to C, B, A respectively, impurity part before the C representative, B represents the higher wood sugar finished product of purity, and A represents the rear impurity part.Its switch into and out of stockline and circular route is all used internally piloted valve (11), (12) control, and a pump (10) is arranged in circulation route, is used for the operation of circulation step.Total system is incubated with chuck, guarantees that bed is constant between the temperature of setting.Complete assembly is according to its running status of PLC time variable control, thus the separation of realization xylose mother liquid.
Adopting sequential simulated moving bed tripping device that xylose mother liquid is separated among the present invention, is to adopt discontinuous charging and discharging, and the mode of discontinuous recycle to extinction liquid stream is carried out, and on traditional SMB basis, its each step is divided into three sub-stepping row:
1. charging, extraction step: advance raw material and eluent, extract anterior impurity out
2. recycle to extinction goes on foot: all chromatogram column systems carry out recycle to extinction
3. wash-out goes on foot: advance eluent, wash out rear portion impurity
By separating, anterior impurity and the rear portion impurity part that can excise the chromatogram elution curve are isolated the wood sugar that is positioned at middle portion, to reach the purpose of purifying xylose mother liquor.
Adopt commercially available chromatographic separation resin as stationary phase in the chromatographic column of the sequential simulated moving bed tripping device of the present invention, need not special preparation, employing water is eluent, and separation temperature is 30～90 ℃.
Xylose mother liquid obtains three class components through separation after entering system's separation, and a class is preceding impurity part, based on glucose; A middle class is for being rich in the component of wood sugar (wood sugar purity 80～100%); Another kind of is the rear impurity part, and pectinose is in this enrichment.
Positively effect of the present invention is: 1, sequential simulated moving bed employing commercially available, and in a large number industrial applications, through the calcium type chromatographic separation resin that prolonged application tests, need not special preparation.2, utilize sequential simulated moving bed tripping device, the wood sugar that can will be positioned at the elution curve middle part is better separated, and obtains more purity of xylose finished product, to the purification particularly advantageous of target product at the elution curve middle part.3, adopt sequential simulated moving bed tripping device to separate xylose mother liquid, need not to remove the glucose composition in the xylose mother liquid, simplified production process.4, the full-automatic control of production process, labour intensity is low, and production site is little.5, production cost is low, adopts discontinuous formula to separate, and eluent can be fully used, and separation only needs water and a small amount of; 6, when reaching equal separation efficiency, required chromatographic column number is than traditional simulation moving-bed lacking.7, do not use any chemical in the production process, produce without any polluting.
Description of drawings
The present invention is further described for the contrast drawings and Examples below:
Accompanying drawing 1 is the sequential simulated moving bed tripping device structural representation of the present invention;
Impurity jar before 1～6 chromatographic column, 7 charging stock tanks, 9 fresh feed pumps, 10 recycle pumps, 11 discharging autocontrol switch valves, 12 circular route autocontrol switch valves, 13 discharge tanks, F raw material, D eluent, A rear impurity jar, B product jar, the C among the figure.
Embodiment:
Utilize the device as accompanying drawing 1 flow process, there are 6 chromatographic columns (1-6 number) in system, and the chromatographic separation of packing in chromatographic column resin, resin are commercially available industrial calcium type strong acidic ion resin.Separation temperature is 70 ℃, pressure 0.3MPa.Charge raw material concentration is 50%, and wherein wood sugar accounts for 62.0%, and glucose accounts for 8.2%, and pectinose accounts for 22.6%, and other assorted sugar accounts for 7.2%.Pure water is an eluent.
Technical process is operated by following program:
The first step: charging, extraction step: eluent water enters post 1 top, goes out product B from post 2 bottoms; Advance separate raw materials from post 4 tops, go out effluent liquid C from post 5 bottoms.
Second step: circulation step: stop charging and discharging, system's recycle to extinction, the liquid flow path direction is to post 6 by post 1.
The 3rd step: the wash-out step: eluent water enters post 2 tops, goes out effluent liquid A by post 1 bottom.
Repeat above three steps in order, different is that in this first step with in the 3rd step, the charging and discharging position moves to next post.Procedure operation all like this later on, the liquid flow path direction is downward all the time in the post.
After system reached balance, the discharging situation that obtains was as follows:
(1) preceding impurity portion C: concentration 5%, glucose accounts for 75.6%;
(2) wood sugar finished product part B: concentration 31.5%, wood sugar accounts for 90.2%;
(3) rear impurity part A: concentration 7.5%, pectinose accounts for 85.8%.
Claims (3)
1, utilize the method for sequential simulated moving bed separation xylose mother liquid, it is characterized in that separating technology comprises: 1) sequential simulated moving bed isolation technique is separated xylose mother liquid, and adopting water is eluent, and separation temperature is 30～90 ℃; 2) xylose mother liquid is well separated by the chromatographic column of chromatographic separation resin being housed, making the wood sugar that is positioned at the elution curve middle part, made the xylose solution of higher degree; 3) sequential simulated moving bed tripping device separates xylose mother liquid, adopts calcium type strong acidic ion resin as separation resin.
2. according to the described method of utilizing sequential simulated moving bed separation xylose mother liquid of claim 1, the program that it is characterized in that sequential simulated moving bed separation xylose mother liquid is, on the basis of traditional analog moving-bed schedule of operation, its each step is divided into three substeps:
First substep: charging, extraction step: advance raw material and eluent, extract anterior impurity out
Second substep: the recycle to extinction step: all chromatogram column system carries out recycle to extinction
The 3rd substep: wash-out step: advance eluent, wash out rear portion impurity
3. according to the described method of utilizing sequential simulated moving bed separation xylose mother liquid of claim 1, it is characterized in that sequential simulated moving bed is the device of forming with 4-10 chromatographic column, chromatographic column is connected in series, the loop system that becomes head and the tail to connect, import at every root chromatogram column all has charging, water-in, outlet at every root chromatogram column all has three classes to flow out component, be that every column top all has eluent D and raw material F feeding line, the autocontrol switch valve is all arranged on the pipeline, every post bottom is equipped with effluent liquid A, B, C flows out pipeline, the autocontrol switch valve is set on the pipeline, also is provided with internally piloted valve on the intercolumniation circular route, lock out operation follow procedure control automatically carries out.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100141758A CN101284849A (en) | 2007-04-13 | 2007-04-13 | Process for purifying xylose mother liquor by sequential simulated moving bed |
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| CNA2007100141758A CN101284849A (en) | 2007-04-13 | 2007-04-13 | Process for purifying xylose mother liquor by sequential simulated moving bed |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928305A (en) * | 2010-05-31 | 2010-12-29 | 黑龙江省农产品加工工程技术研究中心 | Method for purifying xylo-oligosaccharide by adsorption and separation by simulated moving bed |
| CN101857886B (en) * | 2009-04-09 | 2012-12-26 | 华北制药康欣有限公司 | Method for preparing xylitol and co-producing L-arabinose |
| CN102850408A (en) * | 2012-09-12 | 2013-01-02 | 黑龙江八一农垦大学 | Method for preparing xylose and arabinose by using simulated moving chromatography |
| CN102964393A (en) * | 2012-11-30 | 2013-03-13 | 安徽丰原发酵技术工程研究有限公司 | Method for producing xylose by use of xylose mother liquid |
| CN104498559A (en) * | 2014-11-28 | 2015-04-08 | 山东福田药业有限公司 | Clean production process of xylose |
| CN104587706A (en) * | 2014-12-11 | 2015-05-06 | 山东福田药业有限公司 | Method for refining xylose hydrolysate |
| CN109503676A (en) * | 2018-11-27 | 2019-03-22 | 浙江华康药业股份有限公司 | A method of preparing xylitol and mixing molasses from xylose mother liquid |
| CN111705168A (en) * | 2020-07-08 | 2020-09-25 | 江南大学 | Method for purifying xylose hydrolysate by desalting with three zones with simulated moving bed |
| CN113813646A (en) * | 2021-10-20 | 2021-12-21 | 河北乐开节能科技股份有限公司 | Chromatographic separation device and separation method for desalting and decoloring |
| CN113893578A (en) * | 2021-09-08 | 2022-01-07 | 四川雅华生物有限公司 | Separation and purification system and process method of hydrolysate |
| CN114163406A (en) * | 2021-12-15 | 2022-03-11 | 浙江新和成股份有限公司 | Method for recovering vitamin C from vitamin C mother liquor |
| CN114276389A (en) * | 2021-11-15 | 2022-04-05 | 欧尚元(天津)有限公司 | Method and system for purifying xylose by valve array type continuous chromatography |
-
2007
- 2007-04-13 CN CNA2007100141758A patent/CN101284849A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857886B (en) * | 2009-04-09 | 2012-12-26 | 华北制药康欣有限公司 | Method for preparing xylitol and co-producing L-arabinose |
| CN101928305A (en) * | 2010-05-31 | 2010-12-29 | 黑龙江省农产品加工工程技术研究中心 | Method for purifying xylo-oligosaccharide by adsorption and separation by simulated moving bed |
| CN102850408A (en) * | 2012-09-12 | 2013-01-02 | 黑龙江八一农垦大学 | Method for preparing xylose and arabinose by using simulated moving chromatography |
| CN102850408B (en) * | 2012-09-12 | 2015-06-17 | 黑龙江八一农垦大学 | Method for preparing xylose and arabinose by using simulated moving chromatography |
| CN102964393A (en) * | 2012-11-30 | 2013-03-13 | 安徽丰原发酵技术工程研究有限公司 | Method for producing xylose by use of xylose mother liquid |
| CN102964393B (en) * | 2012-11-30 | 2014-12-03 | 安徽丰原发酵技术工程研究有限公司 | Method for producing xylose by use of xylose mother liquid |
| CN104498559A (en) * | 2014-11-28 | 2015-04-08 | 山东福田药业有限公司 | Clean production process of xylose |
| CN104587706A (en) * | 2014-12-11 | 2015-05-06 | 山东福田药业有限公司 | Method for refining xylose hydrolysate |
| CN109503676A (en) * | 2018-11-27 | 2019-03-22 | 浙江华康药业股份有限公司 | A method of preparing xylitol and mixing molasses from xylose mother liquid |
| CN111705168A (en) * | 2020-07-08 | 2020-09-25 | 江南大学 | Method for purifying xylose hydrolysate by desalting with three zones with simulated moving bed |
| CN113893578A (en) * | 2021-09-08 | 2022-01-07 | 四川雅华生物有限公司 | Separation and purification system and process method of hydrolysate |
| CN113813646A (en) * | 2021-10-20 | 2021-12-21 | 河北乐开节能科技股份有限公司 | Chromatographic separation device and separation method for desalting and decoloring |
| CN114276389A (en) * | 2021-11-15 | 2022-04-05 | 欧尚元(天津)有限公司 | Method and system for purifying xylose by valve array type continuous chromatography |
| CN114276389B (en) * | 2021-11-15 | 2023-11-07 | 欧尚元智能装备有限公司 | Method and system for purifying xylose by valve array type continuous chromatography |
| CN114163406A (en) * | 2021-12-15 | 2022-03-11 | 浙江新和成股份有限公司 | Method for recovering vitamin C from vitamin C mother liquor |
| CN114163406B (en) * | 2021-12-15 | 2023-03-31 | 浙江新和成股份有限公司 | Method for recovering vitamin C from vitamin C mother liquor |
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