CN105669419B - The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution - Google Patents
The method of saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution Download PDFInfo
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Abstract
The present invention relates to the method for saccharic acid in sequential simulated moving bed separating corn stalk acid hydrolysis solution, it is specially：Maize straw acid hydrolysis solution is separated by sequential type simulated moving bed chromatography equipment, separation phase, the series connection of 8 root chromatogram columns, extract liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid is injected in the 5th post in the 4th post, successively circulate operation；Desorption phase, strippant is entered on the 1st post top, sulfuric acid solution is released under the 6th post；Desorption phase is fed, strippant is entered on the 1st post top, the 5th root chromatogram column top enters the maize straw acid hydrolysis solution, releases sugar juice under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column；Isolated sulfuric acid solution concentration is 210mg/mL~320mg/mL, and sugar juice concentration is 20mg/mL~41mg/mL；Sulfuric acid solution concentration and recovery；Sugar juice filtering and concentrating.Sulfuric acid concentration after present invention separation is high, and sugar juice concentration is high, solves retrieval of sulfuric acid problem in maize straw recycling, and cost is low.
Description
First, technical field
The present invention relates to the isolation technics of sulfuric acid and liquid glucose in maize straw acid hydrolysis solution, and in particular to sequential simulated
The method of saccharic acid in moving bed separating corn stalk acid hydrolysis solution.
2nd, background technology
China is a large agricultural country, and all kinds of agronomic crop fibre resource very abundants, only stalk one are annual just up to 700,000,000 tons
More than, wherein about 2.2 hundred million tons of maize straw.But at present in addition to the feed that sub-fraction is used as ruminant, remainder it is more with
Fuel is burnt up, and causes Air seriously polluted.Contain substantial amounts of cellulose and hemicellulose in maize straw, number of ways can be passed through
Convert saccharogenesis, the source as fermentation industry low cost feedstock.
Maize straw is refined sugar based on sulphuric acid hydrolysis and enzyme edman degradation Edman, wherein, because enzyme cost is high, low production efficiency,
So enzyme edman degradation Edman is not used for the hydrolysis application of maize straw on a large scale.Sulphuric acid hydrolysis maize straw in technological process, be produced into
All had a clear superiority on this and total reducing sugar yield, can large-scale application in the pretreatment of maize straw.But sulfuric acid in this method
The problem for being always puzzlement Business survival and development is removed, using ion-exchange-resin process to the sulfuric acid in corn stalk hydrolysis
Adsorbed, the problem of cost is high, efficiency is low be present, while the flushing liquor discharge of regenerating ion exchange resin can cause largely
Pollution.Therefore, effectively the sulfuric acid in maize straw acid hydrolysis solution is reclaimed, and controls its cost recovery, while by corn
The utilization that stalk acid hydrolysis solution carries out high added value is the main research during maize straw recycles.
Chinese patent 201210005679.4 discloses a kind of sugar of lignocellulose hydrolysate, acid, salt separation method, Wen Zhong
Refer to and saccharic acid separation is carried out to hydrolyzate using Simulation moving bed, inorganic acid, salt be fast component during separation, and sugar, acetic acid are slow group
Point, it is that acetic acid is not completely separable with sugar, and do not list specific Simulation moving bed separating technology and condition.
Li Xun etc. reports the research [solar energy of the saccharic acid in Simulation moving bed ion exclusion chromatography separation hydrolyzate
Report, 2005,29 (6):747-751], its main contents is that biomass hydrolysate is carried out using the area's continuous analog moving bed of 8 post 4
Saccharic acid is separated, and the concentration of sulfuric acid is 12%~15% in raw material, and sugared concentration is 1.5%~2.0% in extract solution, and the simulation of use is moved
Bed separating technology is traditional 4 area's patterns, and the pattern is continuous feed, continuous elution, and it is shorter to act on the time of material separation, deposits
In low production efficiency, the problems such as solution cost recovery is high.Due to this limitation, amount of dry matter is difficult to improve in raw material, if improving
Product purity and yield after separating can be caused to decline.
3rd, the content of the invention
It is this 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
The method of saccharic acid is applied to solve traditional analog moving bed separation work in sequential simulated moving bed separating corn stalk acid hydrolysis solution
Skill carries out the problem of high solution cost recovery existing for saccharic acid separation, low production efficiency.
To achieve these goals, the concrete technical scheme that the present invention uses is as follows：This sequential simulated moving bed point
From the method for saccharic acid in maize straw acid hydrolysis solution, using maize straw acid hydrolysis solution as raw material, using sequential simulated moving bed separation
Equipment separates sulfuric acid and liquid glucose, sulfuric acid content 500mg/ml~700mg/ml, liquid glucose content 60mg/ml in maize straw acid hydrolysis solution
~80mg/ml；It is specific as follows：
A, sequential simulated moving bed separation：The maize straw acid hydrolysis solution is set by sequential type simulated moving bed chromatography
Standby to be separated, separation process a cycle includes 8 steps, and each step includes three phases, and the first stage is separation phase, and 8
Root chromatogram column is connected in series, and is extracted liquid in post out by the circulating pump under the 3rd post and is injected the 4th post, liquid in the 4th post
Body is injected in the 5th post, back and forth carries out circulate operation successively；Second stage is desorption phase, enters desorption on the 1st post top
Agent, sulfuric acid solution is released under the 6th post；Phase III is charging desorption phase, enters strippant on the 1st post top, the 5th
Chromatographic column top enters the maize straw acid hydrolysis solution, and sugar juice is released under the 1st post, and it is molten to release sulfuric acid under the 6th root chromatogram column
Liquid.After the completion of these three stages, the charging aperture and discharging opening of desorption phase and charging desorption phase are all moved rearwards one successively
Chromatographic column, the three phases for carrying out each step being repeated, 8 steps are completed to be that 8 root chromatogram column rotation, one week i.e. a cycle terminates,
Next next cycle is entered, method and first cycle phase are same, circulate successively, until separation process reaches stable state.Separation
Obtained sulfuric acid solution concentration is 210mg/mL~320mg/mL, purity is 93%~98%, sugar juice concentration be 20mg/mL~
41mg/mL, purity 93%~96%；
B, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through a steps carry out rotary evaporation processing, temperature 50 C~
65 DEG C, concentrate is obtained, concentrate concentration is 500mg/mL~550mg/mL；
C, sugar juice filters：A steps are made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
D, sugar juice concentrates：Sugar juice is made in step c and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid.
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, crushed 40 mesh sieves, weighs certain mass
Maize straw, according to solid-liquid ratio 1:The sulfuric acid solution of 50 ratio addition volumetric concentration 3%, is placed in Microwave Extraction Apparatus, adjustment is micro-
Wave power 700W, 80 DEG C of temperature, 153min is reacted, obtains maize straw acid hydrolysis solution；
Second step, with filter paper maize straw acid hydrolysis solution made from the first step is filtered, obtain clarifying dark brown liquid, and profit
Sulfuric acid content 500mg/ml~700mg/ml in solution, liquid glucose content 60mg/ml~80mg/ are concentrated into Rotary Evaporators
ml。
The sulphuric acid concentration liquid that step b is obtained in such scheme dilutes to obtain the sulfuric acid solution of volumetric concentration 3%, is recycled and reused for
In the first step prepared by maize straw acid hydrolysis solution.
In such scheme in sequential simulated moving bed separation, adsorbent is cationic ion-exchange resin UBK08, IR120H+、IR118H+、IR120Na+Or AMBERJET C1H+Any one of；Strippant is deionized water, and separation temperature is 50 DEG C
~55 DEG C, first stage internal circulating load is 410~550mL；Second stage, strippant flow are 23~45mL/min, desorption time
For 110~160s；Phase III, strippant flow are 30~45mL/min, and inlet amount is 35~50mL/min, charging and desorption
Time is 120~180s.
Beneficial effect：
1st, core technology of the invention is sulfuric acid and liquid glucose skill in sequential simulated moving bed separating corn stalk acid hydrolysis solution
Art, to separate sulfuric acid with liquid glucose compared with high separation, raw materials used sulfuric acid concentration reaches 50%~80%, and sugar concentration is 6%~
8%, 3~5 times are higher by compared with the sulfuric acid concentration in biomass material used in Li Xun etc., the treating capacity of technique significantly increases；Li Xun etc. is pressed
According to technique [solar energy journal, 2005,29 (6) of its report:747-751] separated after sulfuric acid concentration be up to 7%, sugar
Liquid concentration is up to 2%, and sulfuric acid and liquid glucose purity and yield reach 93%.Present invention process act on material separation time compared with
Long, the sulfuric acid concentration after separation is up to 31.8%, purity up to 97.8%, and yield is up to up to 98%, sugar juice concentration
4.05%th, purity is up to 95%, and yield is up to 97%；Therefore, this technique can save mass energy, and sulphur in subsequent concentration processing
The yield and purity of acid and liquid glucose are higher, solve the recovery problem of sulfuric acid in maize straw recycling, have process letter
Just, the distinct characteristic such as process costs saving.
2nd, the present invention is separated using sulfuric acid in the sequential simulated moving bed acid hydrolysis solution to maize straw and liquid glucose, is obtained
The yield of sulfuric acid solution is 93%~98%, and sugar juice yield is 94%~97%.Good separating effect, high income, it is easy to industrial metaplasia
Production amplification.
4th, embodiment
The present invention is described further below：
Embodiment 1：
The method of saccharic acid is as follows in this sequential simulated moving bed separating corn stalk acid hydrolysis solution：
A, the preparation of maize straw acid hydrolysis solution：Maize straw is dried, crushed 40 mesh sieves, weighs 2g corn stalk powders,
The sulfuric acid solution 100mL of volumetric concentration 3% is added, is placed in Microwave Extraction Apparatus, adjusts microwave power 700W, 80 DEG C of temperature, reaction
153min, obtain maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution made from a steps is filtered with filter paper, obtains clarifying dark brown liquid, and utilize rotation
Evaporimeter is concentrated into sulfuric acid concentration 519.4mg/mL in solution, sugar concentration 61.49mg/mL.
C, sequential simulated moving bed separation：Maize straw acid hydrolysis solution after processing passes through sequential type simulated moving bed chromatography
Equipment is separated, and adsorbent is cationic ion-exchange resin UBK08；Strippant is deionized water, and separation temperature is 50 DEG C, separation
Process a cycle includes 8 steps, and each step includes three phases, and the first stage is separation phase, and the series connection of 8 root chromatogram columns connects
Connect, extract liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid injects the 5th post in the 4th post
In, circulate operation, internal circulating load 410mL are back and forth carried out successively；Second stage is desorption phase, enters solution on the 1st post top
Vapor, sulfuric acid solution is released under the 6th post, strippant flow is 23.5mL/min, desorption time 112s；Phase III be into
Expect desorption phase, strippant is entered on the 1st post top, the 5th root chromatogram column top enters maize straw acidolysis obtained by b step
Liquid, sugar juice being released under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column, strippant flow is 30.5mL/min, charging
Measure as 42.2mL/min, charging and desorption time are 180s.After the completion of these three stages, desorption phase and charging desorption phase
Charging aperture and discharging opening are all moved rearwards a chromatographic column successively, repeat the three phases for carrying out each step, and the completion of 8 steps is
8 root chromatogram column rotations one week are that a cycle terminates, and next into next cycle, method and first cycle phase are same, according to
Secondary circulation, until separation process reaches stable state.Isolated sulfuric acid solution concentration is 230mg/mL, purity 93.1%, yield
For 93.5%, sugar juice concentration is 24.8mg/mL, purity 95.2%, yield 94.2%；
D, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through step c carry out rotary evaporation processing, 55 DEG C of temperature,
Concentrate is obtained, then is repeated maize straw acidolysis experiment；
E, sugar juice filters：Step c is made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
F, sugar juice concentrates：Sugar juice is made in step e and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid；
Embodiment 2：
The method of saccharic acid is as follows in this sequential simulated moving bed separating corn stalk acid hydrolysis solution：
A, the preparation of maize straw acid hydrolysis solution：Maize straw is dried, crushed, weighs certain mass maize straw, according to
Solid-liquid ratio 1:50 ratios add the sulfuric acid solution of volumetric concentration 3%, are placed in Microwave Extraction Apparatus, adjust microwave power 700W, temperature
80 DEG C, 153min is reacted, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution made from a steps is filtered with filter paper, obtains clarifying dark brown liquid, and utilize rotation
Evaporimeter is concentrated into sulfuric acid concentration 562.3mg/mL in solution, sugar concentration 65.8mg/mL.
C, sequential simulated moving bed separation：Maize straw acid hydrolysis solution after processing passes through sequential type simulated moving bed chromatography
Equipment is separated, and adsorbent is cationic ion-exchange resin IR120H+；Strippant is deionized water, and separation temperature is 55 DEG C, point
Include 8 steps from process a cycle, each step includes three phases, and the first stage is separation phase, and the series connection of 8 root chromatogram columns connects
Connect, extract liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid injects the 5th post in the 4th post
In, circulate operation, internal circulating load 435mL are back and forth carried out successively；Second stage is desorption phase, enters solution on the 1st post top
Vapor, sulfuric acid solution is released under the 6th post, strippant flow is 25.1mL/min, desorption time 123s；Phase III be into
Expect desorption phase, strippant is entered on the 1st post top, the 5th root chromatogram column top enters maize straw acidolysis obtained by b step
Liquid, sugar juice being released under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column, strippant flow is 30.1mL/min, charging
Measure as 43.5mL/min, charging and desorption time are 179s.After the completion of these three stages, desorption phase and charging desorption phase
Charging aperture and discharging opening are all moved rearwards a chromatographic column successively, repeat the three phases for carrying out each step, and the completion of 8 steps is
8 root chromatogram column rotations one week are that a cycle terminates, and next into next cycle, method and first cycle phase are same, according to
Secondary circulation, until separation process reaches stable state.Isolated sulfuric acid solution concentration is 241mg/mL, purity 94%, and yield is
95.2%, sugar juice concentration is 26.3mg/mL, purity 93.5%, yield 94.6%；
D, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through step c carry out rotary evaporation processing, 55 DEG C of temperature,
Concentrate is obtained, then is repeated maize straw acidolysis experiment；
E, sugar juice filters：Step c is made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
F, sugar juice concentrates：Sugar juice is made in step e and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid；
Embodiment 3：
The method of saccharic acid is as follows in this sequential simulated moving bed separating corn stalk acid hydrolysis solution：
A, the preparation of maize straw acid hydrolysis solution：Maize straw is dried, crushed, weighs certain mass maize straw, according to
Solid-liquid ratio 1:50 ratios add the sulfuric acid solution of volumetric concentration 3%, are placed in Microwave Extraction Apparatus, adjust microwave power 700W, temperature
80 DEG C, 153min is reacted, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution made from a steps is filtered with filter paper, obtains clarifying dark brown liquid, and utilize rotation
Evaporimeter is concentrated into sulfuric acid concentration 616.1mg/mL in solution, sugar concentration 70.2mg/mL.
C, sequential simulated moving bed separation：Maize straw acid hydrolysis solution after processing passes through sequential type simulated moving bed chromatography
Equipment is separated, and adsorbent is cationic ion-exchange resin IR118H+；Strippant is deionized water, and separation temperature is 55 DEG C, point
Include 8 steps from process a cycle, each step includes three phases, and the first stage is separation phase, and the series connection of 8 root chromatogram columns connects
Connect, extract liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid injects the 5th post in the 4th post
In, circulate operation, internal circulating load 428mL are back and forth carried out successively；Second stage is desorption phase, enters solution on the 1st post top
Vapor, sulfuric acid solution is released under the 6th post, strippant flow is 24.5mL/min, desorption time 112s；Phase III be into
Expect desorption phase, strippant is entered on the 1st post top, the 5th root chromatogram column top enters maize straw acidolysis obtained by b step
Liquid, sugar juice being released under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column, strippant flow is 34.5mL/min, charging
Measure as 36.4mL/min, charging and desorption time are 127s.After the completion of these three stages, desorption phase and charging desorption phase
Charging aperture and discharging opening are all moved rearwards a chromatographic column successively, repeat the three phases for carrying out each step, and the completion of 8 steps is
8 root chromatogram column rotations one week are that a cycle terminates, and next into next cycle, method and first cycle phase are same, according to
Secondary circulation, until separation process reaches stable state.Isolated sulfuric acid solution concentration is 318.6mg/mL, purity 97.8%, is received
Rate is 98%, and sugar juice concentration is 40.5mg/mL, purity 95%, yield 97%；
D, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through step c carry out rotary evaporation processing, 55 DEG C of temperature,
Concentrate is obtained, then is repeated maize straw acidolysis experiment；
E, sugar juice filters：Step c is made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
F, sugar juice concentrates：Sugar juice is made in step e and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid；
Embodiment 4：
The method of saccharic acid is as follows in this sequential simulated moving bed separating corn stalk acid hydrolysis solution：
A, the preparation of maize straw acid hydrolysis solution：Maize straw is dried, crushed, weighs certain mass maize straw, according to
Solid-liquid ratio 1:50 ratios add the sulfuric acid solution of volumetric concentration 3%, are placed in Microwave Extraction Apparatus, adjust microwave power 700W, temperature
80 DEG C, 153min is reacted, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution made from a steps is filtered with filter paper, obtains clarifying dark brown liquid, and utilize rotation
Evaporimeter is concentrated into sulfuric acid concentration 546.8mg/mL in solution, sugar concentration 63.4mg/mL.
C, sequential simulated moving bed separation：Maize straw acid hydrolysis solution after processing passes through sequential type simulated moving bed chromatography
Equipment is separated, and adsorbent is cationic ion-exchange resin IR120Na+；Strippant is deionized water, and separation temperature is 52 DEG C,
Separation process a cycle includes 8 steps, and each step includes three phases, and the first stage is separation phase, and 8 root chromatogram columns are connected
Connection, extract liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid injects the 5th in the 4th post
In post, circulate operation, internal circulating load 430mL are back and forth carried out successively；Second stage is desorption phase, is entered on the 1st post top
Strippant, sulfuric acid solution is released under the 6th post, strippant flow is 25.8mL/min, desorption time 131s；Phase III is
Desorption phase is fed, strippant is entered on the 1st post top, the 5th root chromatogram column top enters maize straw acidolysis obtained by b step
Liquid, sugar juice being released under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column, strippant flow is 35.6mL/min, charging
Measure as 40.5mL/min, charging and desorption time are 156s.After the completion of these three stages, desorption phase and charging desorption phase
Charging aperture and discharging opening are all moved rearwards a chromatographic column successively, repeat the three phases for carrying out each step, and the completion of 8 steps is
8 root chromatogram column rotations one week are that a cycle terminates, and next into next cycle, method and first cycle phase are same, according to
Secondary circulation, until separation process reaches stable state.Isolated sulfuric acid solution concentration is 214mg/mL, purity 95.2%, yield
For 95.2%, sugar juice concentration is 23.4mg/mL, purity 94.6%, yield 94.8%；
D, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through step c carry out rotary evaporation processing, 55 DEG C of temperature,
Concentrate is obtained, then is repeated maize straw acidolysis experiment；
E, sugar juice filters：Step c is made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
F, sugar juice concentrates：Sugar juice is made in step e and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid；
Embodiment 5：
The method of saccharic acid is as follows in this sequential simulated moving bed separating corn stalk acid hydrolysis solution：
A, the preparation of maize straw acid hydrolysis solution：Maize straw is dried, crushed, weighs certain mass maize straw, according to
Solid-liquid ratio 1:50 ratios add the sulfuric acid solution of volumetric concentration 3%, are placed in Microwave Extraction Apparatus, adjust microwave power 700W, temperature
80 DEG C, 153min is reacted, obtains maize straw acid hydrolysis solution.
B, maize straw acid hydrolysis solution made from a steps is filtered with filter paper, obtains clarifying dark brown liquid, and utilize rotation
Evaporimeter is concentrated into sulfuric acid concentration 635.4mg/mL in solution, sugar concentration 73.5mg/mL.
C, sequential simulated moving bed separation：Maize straw acid hydrolysis solution after processing passes through sequential type simulated moving bed chromatography
Equipment is separated, and adsorbent is cationic ion-exchange resin AMBERJET C1H+；Strippant is deionized water, and separation temperature is
55 DEG C, separation process a cycle includes 8 steps, and each step includes three phases, and the first stage is separation phase, 8 chromatograms
Post is connected in series, and extracts liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid injects in the 4th post
In 5th post, circulate operation, internal circulating load 550mL are back and forth carried out successively；Second stage is desorption phase, on the 1st post top
Into strippant, sulfuric acid solution is released under the 6th post, strippant flow is 32.5mL/min, desorption time 146s；3rd rank
Section is charging desorption phase, and strippant is entered on the 1st post top, and the 5th root chromatogram column top enters maize straw obtained by b step
Acid hydrolysis solution, sugar juice to be released under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column, strippant flow is 32.5mL/min,
Inlet amount is 41.3mL/min, and charging and desorption time are 162s.After the completion of these three stages, desorption phase and charging desorption rank
The charging aperture and discharging opening of section are all moved rearwards a chromatographic column successively, repeat the three phases for carrying out each step, 8 steps are complete
Terminate into one week i.e. a cycle of i.e. 8 root chromatogram column rotation, next into next cycle, method and first cycle phase
Together, circulate successively, until separation process reaches stable state.Isolated sulfuric acid solution concentration is 264mg/mL, purity is
93.4%, yield 94.3%, sugar juice concentration is 32.4mg/mL, purity 94.9%, yield 96.2%；
D, sulfuric acid solution concentration and recovery：By the sulfuric acid solution obtained through step c carry out rotary evaporation processing, 55 DEG C of temperature,
Concentrate is obtained, then is repeated maize straw acidolysis experiment；
E, sugar juice filters：Step c is made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made
Body；
F, sugar juice concentrates：Sugar juice is made in step e and carries out rotary evaporation processing, temperature is 60~65 DEG C, is made clear
Clear yellow liquid.
Solid-liquid ratio is mass volume ratio in the present invention.
Claims (4)
1. a kind of method of sulfuric acid and liquid glucose in sequential simulated moving bed separating corn stalk acid hydrolysis solution, it is characterised in that：This
The method of sulfuric acid and liquid glucose in the sequential simulated moving bed separating corn stalk acid hydrolysis solution of kind, using maize straw acid hydrolysis solution as original
Material, sulfuric acid and liquid glucose are separated using sequential simulated moving bed separation equipment, sulfuric acid content 500mg/ in maize straw acid hydrolysis solution
Ml~700mg/ml, liquid glucose content 60mg/ml~80mg/ml；It is specific as follows：
A, sequential simulated moving bed separation：The maize straw acid hydrolysis solution is entered by sequential type simulated moving bed chromatography equipment
Row separation, separation process a cycle include 8 steps, and each step includes three phases, and the first stage is separation phase, 8 colors
Spectrum post is connected in series, and extracts liquid in post out injection the 4th post by the circulating pump under the 3rd post, liquid is noted in the 4th post
Enter in the 5th post, back and forth carry out circulate operation successively；Second stage is desorption phase, enters strippant on the 1st post top,
Sulfuric acid solution is released under 6th post；Phase III is charging desorption phase, and strippant, the 5th color are entered on the 1st post top
Spectrum post top enters the maize straw acid hydrolysis solution, releases sugar juice under the 1st post, sulfuric acid solution is released under the 6th root chromatogram column；
After the completion of these three stages, the charging aperture and discharging opening of desorption phase and charging desorption phase are all moved rearwards a chromatogram successively
Post, repeats the three phases for carrying out each step, and 8 steps are completed to be that 8 root chromatogram column rotation, one week i.e. a cycle terminates, connect down
To enter next cycle, method and first cycle phase are same, circulate successively, until separation process reaches stable state；It is isolated
Sulfuric acid solution concentration be 210mg/mL~320mg/mL, purity be 93%~98%, sugar juice concentration is 20mg/mL~41mg/
ML, purity 93%~96%；
B, sulfuric acid solution concentration and recovery：The sulfuric acid solution obtained through a steps is subjected to rotary evaporation processing, temperature 50 C~65
DEG C, concentrate is obtained, concentrate concentration is 500mg/mL~550mg/mL；
C, sugar juice filters：A steps are made into sugar juice to be filtered with micron-rated filter, the yellow liquid of clarification is made；
D, sugar juice concentrates：Sugar juice is made in step c and carries out rotary evaporation processing, temperature is 60~65 DEG C, and clarification is made
Yellow liquid.
2. the side of sulfuric acid and liquid glucose in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 1
Method, 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, crushed 40 mesh sieves, weighs 2g corn stalk powders,
The sulfuric acid solution 100mL of volumetric concentration 3% is added, is placed in Microwave Extraction Apparatus, adjusts microwave power 700W, 80 DEG C of temperature, reaction
153min, obtain maize straw acid hydrolysis solution；
Second step, with filter paper maize straw acid hydrolysis solution made from the first step is filtered, obtain clarifying dark brown liquid, and utilize rotation
Turn evaporimeter and be concentrated into sulfuric acid content 500mg/ml~700mg/ml in solution, liquid glucose content 60mg/ml~80mg/ml.
3. the side of sulfuric acid and liquid glucose in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 2
Method, it is characterised in that：In described sequential simulated moving bed separation, adsorbent be cationic ion-exchange resin UBK08,
IR120H+、IR118 H+、IR120Na+Or AMBERJET C1H+Any one of；Strippant is deionized water, separation temperature
For 50 DEG C~55 DEG C, first stage internal circulating load is 410~550mL；Second stage, strippant flow are 23~45mL/min, solution
The suction time is 110~160s；Phase III, strippant flow are 30~45mL/min, and inlet amount is 35~50mL/min, charging
It is 120~180s with desorption time.
4. the side of sulfuric acid and liquid glucose in sequential simulated moving bed separating corn stalk acid hydrolysis solution according to claim 3
Method, it is characterised in that：The sulphuric acid concentration liquid that described step b is obtained dilutes to obtain the sulfuric acid solution of volumetric concentration 3%, repeats to use
In the first step prepared by maize straw acid hydrolysis solution.
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| 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 |
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