CN105669419A - Method for separation of sugar acid from corn straw acidolysis solution by sequential simulant moving bed - Google Patents

Method for separation of sugar acid from corn straw acidolysis solution by sequential simulant moving bed Download PDF

Info

Publication number
CN105669419A
CN105669419A CN201610010820.8A CN201610010820A CN105669419A CN 105669419 A CN105669419 A CN 105669419A CN 201610010820 A CN201610010820 A CN 201610010820A CN 105669419 A CN105669419 A CN 105669419A
Authority
CN
China
Prior art keywords
soln
acid
sugar
maize straw
hydrolysis solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610010820.8A
Other languages
Chinese (zh)
Other versions
CN105669419B (en
Inventor
曹龙奎
李洪飞
李文杰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Heilongjiang Bayi Agricultural University
Original Assignee
Heilongjiang Bayi Agricultural University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Heilongjiang Bayi Agricultural University filed Critical Heilongjiang Bayi Agricultural University
Priority to CN201610010820.8A priority Critical patent/CN105669419B/en
Publication of CN105669419A publication Critical patent/CN105669419A/en
Application granted granted Critical
Publication of CN105669419B publication Critical patent/CN105669419B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/47Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Saccharide Compounds (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention relates to a method for separation of sugar acid from a corn straw acidolysis solution by a sequential simulant moving bed. The method specifically includes: separation of the corn straw acidolysis solution by sequential simulant moving bed chromatography separation equipment in three stages: a separation stage, which consists of connecting 8 chromatographic columns in series, pumping out the liquid from a third column by a circulating pump therebelow and injecting the liquid into a fourth column, injecting the liquid from the fourth column into a fifth column, and repeating the operation cyclically in order; a desorption stage, which consists of injecting a desorption agent from the upper part of a first column, and discharging a sulfuric acid solution at the bottom of a sixth column; and a feed desorption stage, which consists of injecting a desorption agent from the upper part of the first column, injecting the corn straw acidolysis solution from the upper part of the fifth chromatographic column, discharging a sugar solution from the bottom of the first column, and discharging a sulfuric acid solution from the bottom of the sixth chromatographic column, with the separated sulfuric acid solution having a concentration of 210mg/mL-320mg/mL and the sugar solution having a concentration of 20mg/mL-41mg/mL; concentration and recovery of the sulfuric acid solution; and filtering and concentration of the sugar solution. According to the method provided by the invention, the separated sulfuric acid and sugar solution have a high concentration, thus solving the problems of difficult sulfuric acid recovery and high cost in corn straw reutilization.

Description

The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution
One, technical field
What the present invention relates to is the isolation technique of sulfuric acid and sugar liquid in maize straw acid hydrolysis solution, is specifically related to the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution.
Two, background technology
China is a large agricultural country, and all kinds of agronomic crop fibre resource is very abundant, and only stalk one just reaches more than 700,000,000 tons every year, wherein maize straw about 2.2 hundred million tons. But at present except the feed that sub-fraction is used as ruminating animal, rest part is burnt mainly with fuel, causes Air seriously polluted. Containing a large amount of Mierocrystalline celluloses and hemicellulose in maize straw, transform saccharogenesis by number of ways, as the source of fermentation industry low cost feedstock.
Maize straw is refined sugar based on sulphuric acid hydrolysis and enzyme liberating method, and wherein, because of enzyme class cost height, production efficiency is low, so the not extensive hydrolysis for maize straw of enzyme liberating method is applied. Sulphuric acid hydrolysis maize straw all has clear superiority in technical process, production cost and total reducing sugar receipts rate, can large-scale application in the pre-treatment of maize straw. But the removal of sulfuric acid is a difficult problem for puzzlement Business survival and development in the method always, ion-exchange-resin process is utilized to be adsorbed by the sulfuric acid in corn stalk hydrolysis, there is cost height, inefficient problem, the washing fluid discharge of regenerating ion exchange resin simultaneously can cause a large amount of pollutions. Therefore, effectively being reclaimed by the sulfuric acid in maize straw acid hydrolysis solution, and control its cost recovery, the utilization that maize straw acid hydrolysis solution carries out high added value simultaneously is the main research contents during maize straw recycles.
Chinese patent 201210005679.4 discloses the sugar of a kind of lignocellulose hydrolysate, acid, salt separation method, literary composition is mentioned utilizing and simulation moving-bed hydrolyzed solution is carried out saccharic acid separation, during separation, mineral acid, salt are fast component, sugar, acetic acid are slow component, acetic acid and sugar are not separated completely, and do not list concrete simulation moving-bed separating technology and condition.
Li Xun etc. report the research [solar energy journal of the saccharic acid in simulation moving-bed ion exclusion chromatography separation hydrolyzed solution, 2005, 29 (6): 747-751], biomass hydrolysate is carried out saccharic acid separation for utilizing 8 post 4 district's continuous simulation moving-beds by its main contents, in raw material, the concentration of sulfuric acid is 12%~15%, in extracting solution, sugar concentration is 1.5%~2.0%, the simulation moving-bed separating technology adopted is traditional 4 district's patterns, this pattern is continuously feeding, continuous wash-out, the time acting on separating substances is shorter, there is production efficiency low, the problems such as solution cost recovery height.Due to this kind of restriction, in raw material, amount of dry matter is difficult to improve, if raising can cause being separated rear product purity and the decline of receipts rate.
Three, summary of the invention
Having it is an object of the present invention to provide the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution, in this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is applicable to solve traditional simulation moving-bed separating technology and carries out the solution cost recovery height that saccharic acid separation exists, the problem that production efficiency is low.
In order to realize above-mentioned purpose, the concrete technical scheme that the present invention adopts is as follows: the method for saccharic acid in this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, taking maize straw acid hydrolysis solution as raw material, adopt sequential simulated moving bed separating device separation sulfuric acid and sugar liquid, sulfuric acid content 500mg/ml~700mg/ml, sugar liquid hold-up 60mg/ml~80mg/ml in maize straw acid hydrolysis solution; Specific as follows:
A, sequential simulated moving bed separation: described maize straw acid hydrolysis solution is separated by sequential type simulated moving bed chromatography equipment, sepn process one-period comprises 8 steps, each step comprises three phases, first stage is separation phase, 8 root chromatogram columns are connected in series, being extracted out by liquid in post by the recycle pump being arranged under the 3rd post and inject the 4th post, in the 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post; Phase III is charging desorption phase, enters strippant on the 1st post top, and the 5th root chromatogram column top enters described maize straw acid hydrolysis solution, releases sugar soln, release sulphuric acid soln under the 6th root chromatogram column under the 1st post. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state. The sulphuric acid soln concentration that obtains of separation is 210mg/mL~320mg/mL, purity is 93%~98%, and sugar soln concentration is 20mg/mL~41mg/mL, purity 93%~96%;
B, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through a step is carried out rotary evaporation process, temperature 50 DEG C~65 DEG C, obtains concentrated solution, and concentrated solution concentration is 500mg/mL~550mg/mL;
C, sugar soln filter: filtered by obtained for a step sugar soln micron-rated filter, the yellow liquid of obtained clarification;
D, sugar soln are concentrated: obtained for step c sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification.
The preparation method of maize straw acid hydrolysis solution in such scheme:
The preparation of the first step, maize straw acid hydrolysis solution: maize straw is dried, pulverized 40 order sieves, take certain mass maize straw, the sulphuric acid soln of volumetric concentration 3% is added according to the ratio of solid-liquid ratio 1:50, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution;
2nd step, the maize straw acid hydrolysis solution filtration the first step obtained with filter paper, obtain clarification dark brown liquid, and utilizes Rotary Evaporators to be concentrated to solution sulfuric acid content 500mg/ml~700mg/ml, sugar liquid hold-up 60mg/ml~80mg/ml.
The sulphuric acid concentration liquid dilution that in such scheme, step b obtains obtains the sulphuric acid soln of volumetric concentration 3%, is recycled and reused in the first step prepared by maize straw acid hydrolysis solution.
In separation sequential simulated moving bed in such scheme, sorbent material is Zeo-karb UBK08, IR120H+、IR118H+、IR120Na+Or AMBERJETC1H+In any one; Strippant is deionized water, and separation temperature is 50 DEG C~55 DEG C, and first stage internal circulating load is 410~550mL; Subordinate phase, strippant flow is 23~45mL/min, and desorption time is 110~160s; Phase III, strippant flow is 30~45mL/min, and charging amount is 35~50mL/min, charging and desorption time is 120~180s.
Useful effect:
1, the core technology of the present invention is sulfuric acid and sugar liquid technology in sequential simulated moving bed separating corn stalk acid hydrolysis solution, with relatively high separation, sulfuric acid is separated with sugar liquid, raw materials used sulfuric acid concentration reaches 50%~80%, sugar concentration is 6%~8%, exceeding 3~5 times compared with the sulfuric acid concentration in the biomass materials used such as Li Xun, the treatment capacity of technique obviously increases; The technique [solar energy journal, 2005,29 (6): 747-751] that Li Xun etc. report according to it be separated after sulfuric acid concentration be up to 7%, sugar concentration is up to 2%, sulfuric acid and sugar liquid purity and receipts rate reach 93%. Process acts of the present invention is longer in the time of separating substances, and the sulfuric acid concentration after separation is up to 31.8%, purity can reach 97.8%, and receipts rate can reach 98%, and sugar soln concentration is up to 4.05%, purity can reach 95%, and receipts rate can reach 97%; Therefore, this technique can save a large amount of energy in follow-up concentration, and sulfuric acid is higher with receipts rate and the purity of sugar liquid, solves a recovery difficult problem for sulfuric acid in maize straw recycling, has process simplicity, the characteristic that technique cost savings etc. are distinct.
2, the present invention adopt sequential simulated moving bed to sulfuric acid in maize straw acid hydrolysis solution with sugar liquid be separated, the receipts rate obtaining sulphuric acid soln is 93%~98%, and sugar soln receipts rate is 94%~97%. Good separating effect, receipts rate height, is easy to suitability for industrialized production and amplifies.
Four, embodiment
The present invention is described further below:
Embodiment 1:
In this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is as follows:
The preparation of a, maize straw acid hydrolysis solution: maize straw is dried, pulverized 40 order sieves, take 2g corn stalk powder, add the sulphuric acid soln 100mL of volumetric concentration 3%, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution filtration a step obtained with filter paper, obtain clarification dark brown liquid, and utilize Rotary Evaporators to be concentrated to solution sulfuric acid concentration 519.4mg/mL, sugar concentration 61.49mg/mL.
C, sequential simulated moving bed separation: the maize straw acid hydrolysis solution after process is separated by sequential type simulated moving bed chromatography equipment, sorbent material is Zeo-karb UBK08; Strippant is deionized water, separation temperature is 50 DEG C, sepn process one-period comprises 8 steps, each step comprises three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected in series, by the recycle pump being arranged under the 3rd post liquid in post extracted out and inject the 4th post, in 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively, and internal circulating load is 410mL;Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post, and strippant flow is 23.5mL/min, and desorption time is 112s; Phase III is charging desorption phase, strippant is entered on the 1st post top, 5th root chromatogram column top enters b step gained maize straw acid hydrolysis solution, sugar soln is released under 1st post, sulphuric acid soln is released under 6th root chromatogram column, strippant flow is 30.5mL/min, and charging amount is 42.2mL/min, charging and desorption time is 180s. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state. The sulphuric acid soln concentration that obtains of separation is 230mg/mL, purity is 93.1%, and receipts rate is 93.5%, and sugar soln concentration is 24.8mg/mL, purity 95.2%, and receipts rate is 94.2%;
D, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through step c is carried out rotary evaporation process, temperature 55 DEG C, obtains concentrated solution, then is repeated maize straw acidolysis experiment;
E, sugar soln filter: filtered by obtained for step c sugar soln micron-rated filter, the yellow liquid of obtained clarification;
F, sugar soln are concentrated: obtained for step e sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification;
Embodiment 2:
In this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is as follows:
The preparation of a, maize straw acid hydrolysis solution: maize straw is dried, pulverizes, take certain mass maize straw, the sulphuric acid soln of volumetric concentration 3% is added according to solid-liquid ratio 1:50 ratio, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution filtration a step obtained with filter paper, obtain clarification dark brown liquid, and utilize Rotary Evaporators to be concentrated to solution sulfuric acid concentration 562.3mg/mL, sugar concentration 65.8mg/mL.
C, sequential simulated moving bed separation: the maize straw acid hydrolysis solution after process is separated by sequential type simulated moving bed chromatography equipment, sorbent material is Zeo-karb IR120H+; Strippant is deionized water, separation temperature is 55 DEG C, sepn process one-period comprises 8 steps, each step comprises three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected in series, by the recycle pump being arranged under the 3rd post liquid in post extracted out and inject the 4th post, in 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively, and internal circulating load is 435mL; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post, and strippant flow is 25.1mL/min, and desorption time is 123s; Phase III is charging desorption phase, strippant is entered on the 1st post top, 5th root chromatogram column top enters b step gained maize straw acid hydrolysis solution, sugar soln is released under 1st post, sulphuric acid soln is released under 6th root chromatogram column, strippant flow is 30.1mL/min, and charging amount is 43.5mL/min, charging and desorption time is 179s. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state.The sulphuric acid soln concentration that obtains of separation is 241mg/mL, purity is 94%, and receipts rate is 95.2%, and sugar soln concentration is 26.3mg/mL, purity 93.5%, and receipts rate is 94.6%;
D, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through step c is carried out rotary evaporation process, temperature 55 DEG C, obtains concentrated solution, then is repeated maize straw acidolysis experiment;
E, sugar soln filter: filtered by obtained for step c sugar soln micron-rated filter, the yellow liquid of obtained clarification;
F, sugar soln are concentrated: obtained for step e sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification;
Embodiment 3:
In this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is as follows:
The preparation of a, maize straw acid hydrolysis solution: maize straw is dried, pulverizes, take certain mass maize straw, the sulphuric acid soln of volumetric concentration 3% is added according to solid-liquid ratio 1:50 ratio, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution filtration a step obtained with filter paper, obtain clarification dark brown liquid, and utilize Rotary Evaporators to be concentrated to solution sulfuric acid concentration 616.1mg/mL, sugar concentration 70.2mg/mL.
C, sequential simulated moving bed separation: the maize straw acid hydrolysis solution after process is separated by sequential type simulated moving bed chromatography equipment, sorbent material is Zeo-karb IR118H+; Strippant is deionized water, separation temperature is 55 DEG C, sepn process one-period comprises 8 steps, each step comprises three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected in series, by the recycle pump being arranged under the 3rd post liquid in post extracted out and inject the 4th post, in 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively, and internal circulating load is 428mL; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post, and strippant flow is 24.5mL/min, and desorption time is 112s; Phase III is charging desorption phase, strippant is entered on the 1st post top, 5th root chromatogram column top enters b step gained maize straw acid hydrolysis solution, sugar soln is released under 1st post, sulphuric acid soln is released under 6th root chromatogram column, strippant flow is 34.5mL/min, and charging amount is 36.4mL/min, charging and desorption time is 127s. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state. The sulphuric acid soln concentration that obtains of separation is 318.6mg/mL, purity is 97.8%, and receipts rate is 98%, and sugar soln concentration is 40.5mg/mL, purity 95%, and receipts rate is 97%;
D, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through step c is carried out rotary evaporation process, temperature 55 DEG C, obtains concentrated solution, then is repeated maize straw acidolysis experiment;
E, sugar soln filter: filtered by obtained for step c sugar soln micron-rated filter, the yellow liquid of obtained clarification;
F, sugar soln are concentrated: obtained for step e sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification;
Embodiment 4:
In this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is as follows:
The preparation of a, maize straw acid hydrolysis solution: maize straw is dried, pulverizes, take certain mass maize straw, the sulphuric acid soln of volumetric concentration 3% is added according to solid-liquid ratio 1:50 ratio, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution filtration a step obtained with filter paper, obtain clarification dark brown liquid, and utilize Rotary Evaporators to be concentrated to solution sulfuric acid concentration 546.8mg/mL, sugar concentration 63.4mg/mL.
C, sequential simulated moving bed separation: the maize straw acid hydrolysis solution after process is separated by sequential type simulated moving bed chromatography equipment, sorbent material is Zeo-karb IR120Na+; Strippant is deionized water, separation temperature is 52 DEG C, sepn process one-period comprises 8 steps, each step comprises three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected in series, by the recycle pump being arranged under the 3rd post liquid in post extracted out and inject the 4th post, in 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively, and internal circulating load is 430mL; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post, and strippant flow is 25.8mL/min, and desorption time is 131s; Phase III is charging desorption phase, strippant is entered on the 1st post top, 5th root chromatogram column top enters b step gained maize straw acid hydrolysis solution, sugar soln is released under 1st post, sulphuric acid soln is released under 6th root chromatogram column, strippant flow is 35.6mL/min, and charging amount is 40.5mL/min, charging and desorption time is 156s. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state. The sulphuric acid soln concentration that obtains of separation is 214mg/mL, purity is 95.2%, and receipts rate is 95.2%, and sugar soln concentration is 23.4mg/mL, purity 94.6%, and receipts rate is 94.8%;
D, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through step c is carried out rotary evaporation process, temperature 55 DEG C, obtains concentrated solution, then is repeated maize straw acidolysis experiment;
E, sugar soln filter: filtered by obtained for step c sugar soln micron-rated filter, the yellow liquid of obtained clarification;
F, sugar soln are concentrated: obtained for step e sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification;
Embodiment 5:
In this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, the method for saccharic acid is as follows:
The preparation of a, maize straw acid hydrolysis solution: maize straw is dried, pulverizes, take certain mass maize straw, the sulphuric acid soln of volumetric concentration 3% is added according to solid-liquid ratio 1:50 ratio, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution filtration a step obtained with filter paper, obtain clarification dark brown liquid, and utilize Rotary Evaporators to be concentrated to solution sulfuric acid concentration 635.4mg/mL, sugar concentration 73.5mg/mL.
C, sequential simulated moving bed separation: the maize straw acid hydrolysis solution after process is separated by sequential type simulated moving bed chromatography equipment, sorbent material is Zeo-karb AMBERJETC1H+; Strippant is deionized water, separation temperature is 55 DEG C, sepn process one-period comprises 8 steps, each step comprises three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected in series, by the recycle pump being arranged under the 3rd post liquid in post extracted out and inject the 4th post, in 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively, and internal circulating load is 550mL; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post, and strippant flow is 32.5mL/min, and desorption time is 146s; Phase III is charging desorption phase, strippant is entered on the 1st post top, 5th root chromatogram column top enters b step gained maize straw acid hydrolysis solution, sugar soln is released under 1st post, sulphuric acid soln is released under 6th root chromatogram column, strippant flow is 32.5mL/min, and charging amount is 41.3mL/min, charging and desorption time is 162s. After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state. The sulphuric acid soln concentration that obtains of separation is 264mg/mL, purity is 93.4%, and receipts rate is 94.3%, and sugar soln concentration is 32.4mg/mL, purity 94.9%, and receipts rate is 96.2%;
D, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through step c is carried out rotary evaporation process, temperature 55 DEG C, obtains concentrated solution, then is repeated maize straw acidolysis experiment;
E, sugar soln filter: filtered by obtained for step c sugar soln micron-rated filter, the yellow liquid of obtained clarification;
F, sugar soln are concentrated: obtained for step e sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification.
In the present invention, solid-liquid ratio is mass volume ratio.

Claims (4)

1. the method for saccharic acid in a sequential simulated moving bed separating corn stalk acid hydrolysis solution, it is characterized in that: the method for saccharic acid in this kind of sequential simulated moving bed separating corn stalk acid hydrolysis solution, taking maize straw acid hydrolysis solution as raw material, adopt sequential simulated moving bed separating device separation sulfuric acid and sugar liquid, sulfuric acid content 500mg/ml~700mg/ml, sugar liquid hold-up 60mg/ml~80mg/ml in maize straw acid hydrolysis solution; Specific as follows:
A, sequential simulated moving bed separation: described maize straw acid hydrolysis solution is separated by sequential type simulated moving bed chromatography equipment, sepn process one-period comprises 8 steps, each step comprises three phases, first stage is separation phase, 8 root chromatogram columns are connected in series, being extracted out by liquid in post by the recycle pump being arranged under the 3rd post and inject the 4th post, in the 4th post, liquid injects the 5th post, back and forth carries out cyclical operation successively; Subordinate phase is desorption phase, enters strippant on the 1st post top, releases sulphuric acid soln under the 6th post; Phase III is charging desorption phase, enters strippant on the 1st post top, and the 5th root chromatogram column top enters described maize straw acid hydrolysis solution, releases sugar soln, release sulphuric acid soln under the 6th root chromatogram column under the 1st post;After this three phases completes, the opening for feed of desorption phase and charging desorption phase and discharge port move a chromatographic column all successively backward, repeat the three phases of each step again, it one week is that one-period terminates that 8 steps complete i.e. 8 root chromatogram column rotation, next the next cycle is entered, method is identical with one-period, circulates successively, until sepn process reaches stable state; The sulphuric acid soln concentration that obtains of separation is 210mg/mL~320mg/mL, purity is 93%~98%, and sugar soln concentration is 20mg/mL~41mg/mL, purity 93%~96%;
B, sulphuric acid soln concentration and recovery: the sulphuric acid soln obtained through a step is carried out rotary evaporation process, temperature 50 DEG C~65 DEG C, obtains concentrated solution, and concentrated solution concentration is 500mg/mL~550mg/mL;
C, sugar soln filter: filtered by obtained for a step sugar soln micron-rated filter, the yellow liquid of obtained clarification;
D, sugar soln are concentrated: obtained for step c sugar soln is carried out rotary evaporation process, and temperature is 60~65 DEG C, the yellow liquid of obtained clarification.
2. the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 1, it is characterised in that: the preparation method of described maize straw acid hydrolysis solution:
The preparation of the first step, maize straw acid hydrolysis solution: maize straw is dried, pulverized 40 order sieves, take 2g corn stalk powder, add the sulphuric acid soln 100mL of volumetric concentration 3%, it is placed in microwave extracting instrument, adjustment microwave power 700W, temperature 80 DEG C, reaction 153min, obtains maize straw acid hydrolysis solution;
2nd step, the maize straw acid hydrolysis solution filtration the first step obtained with filter paper, obtain clarification dark brown liquid, and utilizes Rotary Evaporators to be concentrated to solution sulfuric acid content 500mg/ml~700mg/ml, sugar liquid hold-up 60mg/ml~80mg/ml.
3. the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 2, it is characterised in that: in described sequential simulated moving bed separation, sorbent material is Zeo-karb UBK08, IR120H+、IR118H+、IR120Na+Or AMBERJETC1H+In any one; Strippant is deionized water, and separation temperature is 50 DEG C~55 DEG C, and first stage internal circulating load is 410~550mL; Subordinate phase, strippant flow is 23~45mL/min, and desorption time is 110~160s; Phase III, strippant flow is 30~45mL/min, and charging amount is 35~50mL/min, charging and desorption time is 120~180s.
4. the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 3, it is characterized in that: the sulphuric acid concentration liquid dilution that described step b obtains obtains the sulphuric acid soln of volumetric concentration 3%, is recycled and reused in the first step prepared by maize straw acid hydrolysis solution.
CN201610010820.8A 2016-01-09 2016-01-09 The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution Active CN105669419B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610010820.8A CN105669419B (en) 2016-01-09 2016-01-09 The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610010820.8A CN105669419B (en) 2016-01-09 2016-01-09 The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution

Publications (2)

Publication Number Publication Date
CN105669419A true CN105669419A (en) 2016-06-15
CN105669419B CN105669419B (en) 2018-01-26

Family

ID=56299496

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610010820.8A Active CN105669419B (en) 2016-01-09 2016-01-09 The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution

Country Status (1)

Country Link
CN (1) CN105669419B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112979419A (en) * 2021-02-25 2021-06-18 中国科学院过程工程研究所 Method for separating dihydric alcohol by sequential simulated moving bed

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101029060A (en) * 2007-04-04 2007-09-05 牛继星 Hydrolysis for producing high-purity crystallized xylose from corn skin
CN101792822A (en) * 2010-03-30 2010-08-04 天津科技大学 Method for separating and purifying xylose and arabinose from hemicellulose acid hydrolysis liquid
US20100213130A1 (en) * 2009-02-25 2010-08-26 Danisco A/S Separation process
CN102102116A (en) * 2010-12-21 2011-06-22 山东省鲁洲食品集团有限公司 Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues
CN102600640A (en) * 2012-01-09 2012-07-25 中德瑞生物炼制实验室(厦门)有限公司 Method for separating sugar, acid and salt of lignocellulose hydrolysate
CN103992362A (en) * 2014-06-12 2014-08-20 黑龙江八一农垦大学 Method for purifying tagatose by using sequential simulated moving bed chromatography (SSMB)

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101029060A (en) * 2007-04-04 2007-09-05 牛继星 Hydrolysis for producing high-purity crystallized xylose from corn skin
US20100213130A1 (en) * 2009-02-25 2010-08-26 Danisco A/S Separation process
CN101792822A (en) * 2010-03-30 2010-08-04 天津科技大学 Method for separating and purifying xylose and arabinose from hemicellulose acid hydrolysis liquid
CN102102116A (en) * 2010-12-21 2011-06-22 山东省鲁洲食品集团有限公司 Method for preparing high-purity crystalline dextrose from maize peel acid hydrolysis residues
CN102600640A (en) * 2012-01-09 2012-07-25 中德瑞生物炼制实验室(厦门)有限公司 Method for separating sugar, acid and salt of lignocellulose hydrolysate
CN103992362A (en) * 2014-06-12 2014-08-20 黑龙江八一农垦大学 Method for purifying tagatose by using sequential simulated moving bed chromatography (SSMB)

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
李浔等: "模拟移动床离子排斥色谱分离水解液中的糖酸", 《太阳能学报》 *
李良玉等: "模拟移动色谱法纯化葡萄糖母液的技术研究", 《核农学报》 *
聂圣才: "顺序式模拟移动床技术制备结晶果糖的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112979419A (en) * 2021-02-25 2021-06-18 中国科学院过程工程研究所 Method for separating dihydric alcohol by sequential simulated moving bed

Also Published As

Publication number Publication date
CN105669419B (en) 2018-01-26

Similar Documents

Publication Publication Date Title
CN102702144B (en) Method for preparing furan or furfural compound from biomass cellulose
CN102321251B (en) Method for separating xylogen from agricultural waste by using compound ion liquid
CN103951718B (en) A kind of method preparing high-purity gardenoside and crocin with cape jasmine
CN103086889B (en) A kind of method of enzyme catalysis activation leaf of Flos Lonicerae chlorogenic acid extracting
CN112726253A (en) Method for efficiently separating plant fibers by acidic eutectic solvent/metal salt multi-component system
CN101838199A (en) Pleuromutilin solvent extraction process
CN102493246B (en) Method for extracting and separating cellulose from biomass solid waste
CN103088692A (en) Method for selectively separating lignin and cellulose from lignocellulose biomasses
CN103849665A (en) Method for pretreating lignocellulose by using carboxyl functionalized ionic liquid solution
CN105256081A (en) Method for preparing xylose by utilizing distiller's grains of Baijiu
CN105272838A (en) Separating purifying method for ingenol extract
CN110004756A (en) A kind of method of wood fiber biomass component separation
CN105669419A (en) Method for separation of sugar acid from corn straw acidolysis solution by sequential simulant moving bed
CN103265583B (en) A kind of preparation method of stachyose crystal
CN101871020A (en) Method for preparing wood sugar, glucose and lignin with ionic liquid controllable hydrolytic wood fiber raw material
CN105061194A (en) Method for separating lactic acid from lactic acid fermentation liquor by using continuous chromatography technology
CN103755971A (en) Method for extracting lignin of straws by acidic ionic liquid and organic solvent
CN104878056A (en) Method for producing high-purity fructo-oligose
CN107519232A (en) One kind extraction Gueldenstaedtia verna extractive of general flavone and preparation method thereof
CN103333054A (en) Method for extracting resveratrol from grape peel residue with enzymatic method
CN101691587A (en) Detoxification method of wood fibre hydrolysis sugar liquid
CN105255956B (en) The method that stalk hydrolyzate removes fermentation inhibitor
CN105017342A (en) Directional biomass pressurization liquefying method for preparing alkyl glycoside
CN101560239A (en) Production process for extracting saponins from yellow ginger by using solvent catalyzing method
CN102816050A (en) Method for extracting solanesol by activating waste and defective tobacco by enzyme catalysis

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant