CN110527752A - A kind of electrodialysis separating technology of hemicellulose hydrolysate - Google Patents
A kind of electrodialysis separating technology of hemicellulose hydrolysate Download PDFInfo
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- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
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Abstract
The invention discloses a kind of electrodialysis separating technologies of hemicellulose hydrolysate, belong to technical field of xylose production.Three-stage electrodialysis is carried out to hemicellulose hydrolysate, finally obtains the high saline solution of the first order, the high saline solution in the second level, the high saline solution of the third level and the high liquid glucose of the third level, the high saline solution of the first order can direct emission or reuse after being diluted, being neutralized；And after the high saline solution of the third level is concentrated and desalination, enter subsequent processing as the final feed liquid for meeting index (conductance≤4000us/cm, inorganic acid≤0.3%, Xylose Content >=55g/L and xylose purity >=80%) together with the high liquid glucose of the third level；The present invention is applied to desalination, the depickling of hemicellulose hydrolysate, and then reaches removal of impurities to xylose solution, purifying purpose, under the premise of improving xylose quality and production efficiency, it reduces and runs sugar amount, increase economic efficiency, simultaneously, the discharge of difficult sewage is reduced, environmental protection pressure is reduced.
Description
Technical field
The present invention relates to a kind of electrodialysis separating technology of hemicellulose hydrolysate more particularly to it is a kind of use electroosmose process
Remove sulfuric acid in hemicellulose hydrolysate, sodium sulphate and prepare the separating technology of xylose, belong to technical field of xylose production.
Background technique
Hemicellulose is the primary raw material for producing xylose, wherein main during preparing xylose as raw material using hemicellulose
Wanting process includes hydrolysis, decoloration, desalination, deacidification, evaporation, centrifugation and drying etc..Produce xylose specifically comprises the processes of: with hemicellulose
Element is raw material, in a heated condition, sulfuric acid is added into hemicellulose, hemicellulose is xylose by sulphuric acid hydrolysis and other are miscellaneous
Sugar, meanwhile, there are the impurity such as sodium sulphate and sulfuric acid in hydrolyzate；And before rotary process, the xylose of generation is with solution shape
State exists, and therefore, in order to improve xylose quality, needs effectively to remove the impurity such as sodium sulphate, sulfuric acid in hemicellulose hydrolysate.
Currently, in existing separation method, be added generally into hemicellulose hydrolysate salt (such as: calcium oxide, carbonic acid
Barium), acid (such as: sulfuric acid) generate precipitating (calcium sulfate or barium sulfate), with reach the sodium sulphate removed in hemicellulose hydrolysate,
The impurity such as sulfuric acid, but this separating technology is complicated, and controllable difficulty is big, and low efficiency is at high cost, and still there is electrolyte in hydrolyzate
More residual, without being able to satisfy actual process demand.
State Intellectual Property Office disclosed a kind of Publication No. CN109575088A on 04 05th, 2019, and entitled " one
The patent document of the refining methd of xylose in kind hemicellulose hydrolysate ", wherein specific open: it is related to chemical production technical neck
Domain, method includes the following steps: 1), into ultrafiltration membrane, obtaining permeate after hemicellulose hydrolysate removal of impurities；2) it will transmit through liquid
It is separated using nanofiltration membrane, sulfuric acid stays in concentrate, and permeate contains acetic acid and xylose；3) acetic acid and xylose aqueous solution are adopted
It is separated with electrodialysis；4) xylose aqueous solution is directly used in the production of furfural；5) acetic acid carries out extraction and separation with solvent extraction rectifying
Obtain the acetic acid of 98.5% concentration.This method is easy to operate, and obtained xylose aqueous solution is directly used in the production of furfural, and obtains
Mass concentration be 20% or so acetic acid, with solvent extraction rectifier unit carries out extraction and separation can be obtained mass concentration be 98.5%
Acetic acid.In the technique, the sulfuric acid separated returns to hydrolyzing process and continues to use, and effective component is carried out recycling and reusing,
Production cost is saved.
State Intellectual Property Office disclosed a kind of Publication No. CN101792822A on 08 04th, 2010, entitled " from
The patent document of the method for separating-purifying xylose, arabinose in hemicellulose acid hydrolysis liquid ", wherein specific open: separation mentions
Pure step is as follows: (1) hemicellulose hydrolysate for obtaining direct sour water solution is pre-processed through electrodialysis, film filtering and concentrating, high
Pure water progress deoxidation, filtering are spare；(2) enter moving bed imitation chromatogram separation facility by pretreated hemicellulose hydrolysate
It is separated, two kinds of out-feed liquids is obtained after separation；(3) two kinds of out-feed liquids are concentrated with multiple-effect falling film evaporator, decrease temperature crystalline obtains
To xylose, arabinose product.The present invention extracts monosaccharide using moving bed imitation chromatogram separation facility (SSMB) system, will be multiple
Adsorption column is connected into closed loop, changes the inlet and outlet position of each stock material by continuous switch valve, realizes solid, liquid two-phase
Relative movement, carries out the separation and Extraction of different component, its existing ADSORPTION IN A FIXED BED advantage easy to operate, and has moving bed continuous
The ability of operation is suitble to large-scale industrial production.
Although disclosing electroosmose process in above two existing technical literatures to the separating treatment of hemicellulose hydrolysate,
But there is also following technical problems: one, after electrodialysis process, generated waste water environmental pollution is serious, causes environment pressure
Power；Two, it is big to run sugar amount, results in waste of resources, and cause environmental protection pressure；Three, electrodialytic membranes service life is short, in unfavorable work
It is replaced frequently under condition, causes at high cost, and discarded film process is difficult.
Summary of the invention
The present invention is directed to overcome the shortage of prior art, and propose a kind of electrodialysis separating technology of hemicellulose hydrolysate.
In the present invention, three-stage electrodialysis is carried out to the hemicellulose hydrolysate after the pre-treatments such as filtering, decoloration, ultrafiltration, it is final to obtain
To the high saline solution of the first order, the high saline solution in the second level, the high saline solution of the third level and the high liquid glucose of the third level, the high saline solution of the first order through dilution, in
With after can direct emission, it is small to environmental pressure, alternatively, cycling and reutilization, reduce waste, save the cost；And the high saline solution of the third level
(including concentration is 13~15g/L reduced sugar, concentration is 0.5~0.8g/L sulfuric acid, and concentration is 0.5~0.8g/L sodium sulphate, and electric
After leading as 20~30ms/cm) is concentrated and desalination, with the high liquid glucose of the third level together as meeting index (conductance≤4000us/
Cm, refractive power >=7.0, inorganic acid≤0.3%, total acid≤0.4%, content of reducing sugar >=70g/L, Xylose Content >=55g/L and xylose
Purity >=80%) final feed liquid enter subsequent processing.
The present invention is applied to desalination, the depickling of hemicellulose hydrolysate, and then reaches removal of impurities to xylose solution, purifying mesh
, under the premise of improving xylose quality and production efficiency, reduces and run sugar amount (70~80%), increase economic efficiency, meanwhile, subtract
The discharge of few difficult sewage, reduces environmental protection pressure.
In order to achieve the above technical purposes, the following technical solutions are proposed:
A kind of electrodialysis separating technology of hemicellulose hydrolysate, includes the following steps:
1) first order electrodialysis: hemicellulose hydrolysate is passed through to first order electrodialysis system, and is passed through the high saline solution in the second level,
It is acted on through electrodialytic membranes, obtains the high liquid glucose of the first order and the high saline solution of the first order；
2) second level electrodialysis: it will be passed through through the high liquid glucose of the resulting first order of step 1) to second level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high saline solution of the high liquid glucose in the second level and the second level；
3) third level electrodialysis: it will be passed through through the high liquid glucose in the resulting second level of step 2 to third level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high liquid glucose of the third level and the high saline solution of the third level；
4) it post-processes: after the high saline solution concentration of the third level and desalination, being stored in temporary storage tank together with the high liquid glucose of the third level, so
Afterwards, it is injected into ion exchange column, chromatographs, obtain xylose solution.
Further, the hemicellulose hydrolysate refers to: with hemicellulosic material, after sulphuric acid hydrolysis, use is existing
Hemicellulose hydrolysate after the pre-treatments such as mature technology is filtered, decolourizes, ultrafiltration.Wherein, in the hydrolysis of hemicellulose
In liquid, Xylose Content is 70~90g/L, 20~22g/L of sodium sulphate content, 20~25g/L of sulfuric acid content.
Further, in step 1), 2) and 3) in, the electrodialytic membranes is alloy film.
Further, it in the enrichment process of step 4), is concentrated using homogeneous electrodialytic membranes or alloy film, after concentration
The high saline solution conductance of the third level be 200~250 ms/cm.
Further, in step 4) desalination process, desalination is carried out using alloy film, the high saline solution electricity of the third level after desalination
It leads as 3~5 ms/cm.
Further, in the first order electrodialysis system of step 1), hemicellulose hydrolysate feed rate be 40~
50m3/ h, the high saline solution feed rate in the second level are 15~17m3/h；Voltage is 150V, and electric current 100A, temperature is 40~45 DEG C；
The high saline solution discharging flow of the first order is 15~17m3/ h, the high liquid glucose discharging flow of the first order are 40~50m3/h；
In the second level electrodialysis system of step 2, the high liquid glucose feed rate of the first order is 40~50m3/ h, demineralized water charging
Flow is 15~17m3/h；Voltage is 150V, and electric current 100A, temperature is 40~45 DEG C；The high saline solution discharging flow in the second level is
15~17m3/ h, the high liquid glucose discharging flow in the second level are 40~50m3/h；
In the third level electrodialysis system of step 3), the high liquid glucose feed rate in the second level is 40~50m3/ h, demineralized water charging
Flow is 15~17m3/h；Voltage is 150V, and electric current is 75~100A, and temperature is 40~45 DEG C；The high saline solution reactor effluent stream of the third level
Amount is 15~17m3/ h, the high liquid glucose discharging flow of the third level are 40~50m3/h。
Further, in step 1), the high saline solution of the first order include concentration be 17~20g/L reduced sugar, concentration be 35~
45g/L sulfuric acid and concentration are 15~18g/L sodium sulphate；The high liquid glucose of the first order include concentration be 75~90g/L reduced sugar, concentration is
12~14g/L sulfuric acid and concentration are 5~10g/L sodium sulphate；
In step 2, the high saline solution in the second level include concentration be 15~18g/L reduced sugar, concentration is 20~35g/L sulfuric acid and dense
Degree is 15~18g/L sodium sulphate；The high liquid glucose in the second level include concentration be 75~90g/L reduced sugar, concentration is 5~10g/L sulfuric acid
And concentration is 5~10g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 13~15g/L reduced sugar, concentration is 5~8g/L sulfuric acid and concentration
For 5~8g/L sodium sulphate；The high liquid glucose of the third level include concentration be 75~90g/L reduced sugar, concentration is 1~2g/L sulfuric acid and concentration
For 1~2g/L sodium sulphate.
Further, in step 1), the high saline solution conductance of the first order is 150~180ms/cm, and pH is 0.5~1.0, refractive power
It is 5.5~6.5；The high liquid glucose conductance of the first order is 40~50ms/cm, and pH is 1.0~1.3, and refractive power is 8.0~9.0；
In step 2, the high saline solution conductance in the second level is 70~80ms/cm, and pH is 1.0~1.2, and refractive power is 3~4；The second level is high
Liquid glucose conductance is 18~20ms/cm, and pH is 1.8~2.1, and refractive power is 8.0~9.0；
In step 3), the high saline solution conductance of the third level is 20~30ms/cm, and pH is 2~2.2, and refractive power is 1~2；The high sugar of the third level
Liquid conductance is 3~4ms/cm, and pH is 2.2~2.8, and refractive power is 8.0~9.0.
According to standard " xylose of GB/T23532~2009 ", through detecting, the hemicellulose hydrolysate is separated through electrodialysis
Afterwards: conductance≤4000us/cm, light transmittance >=98.0%, refractive power >=7.0,18.5 °~19.5 ° of specific rotatory power, pH is 2.2~2.8；
Content of reducing sugar >=70g/L, Xylose Content >=55g/L, xylose purity >=80%；Inorganic acid≤0.3%, total acid≤0.4%, sulfuric acid
Salt content≤0.005%, ash content≤0.05%, moisture≤0.3%, chloride≤0.005%.
Electrodialysis separation system includes desalination water storage tank and electrodialysis plant, and the electrodialysis plant is three, respectively
First order electrodialysis plant, second level electrodialysis plant and third level electrodialysis plant, first order electrodialysis plant and the second level
Electrodialysis plant connection, forms first order electrodialysis system between first order electrodialysis plant and second level electrodialysis plant；The
Second level electrodialysis plant is connect with desalination water storage tank, and second level electric osmose is formed between desalination water storage tank and second level electrodialysis plant
Analysis system；Second level electrodialysis plant is connect with third level electrodialysis plant, and third level electrodialysis plant and desalination water storage tank connect
It connects, forms third level electrodialysis system between desalination water storage tank and third level electrodialysis plant.
Further, the first order electrodialysis plant feed inlet is connected with the delivery pipe of conveying hemicellulose hydrolysate, the
The high liquid glucose outlet of level-one electrodialysis plant is connect by delivery pipe with second level electrodialysis plant feed inlet, second level electrodialysis dress
It sets high saline solution outlet to connect by delivery pipe with first order electrodialysis plant, electrodialysis plant high liquid glucose outlet in the second level passes through defeated
Pipe is sent to connect with third level electrodialysis plant feed inlet；The high liquid glucose outlet of third level electrodialysis plant is connected with temporarily by delivery pipe
Tank is deposited, the high saline solution outlet of third level electrodialysis plant is connect by delivery pipe with temporary storage tank.
Further, enrichment facility is additionally provided between the high saline solution outlet of the third level electrodialysis plant and temporary storage tank and take off
Salt device, the high saline solution outlet of third level electrodialysis plant are connect with enrichment facility, and enrichment facility is connect with desalter, desalination dress
It sets and is connect with temporary storage tank, temporary storage tank is connected with ion exchange column.
Further, the electrodialysis separation system further includes thinning tank and neutralizing tank, and first order electrodialysis plant is with high salt
Liquid outlet is connect by delivery pipe with thinning tank, and thinning tank is connect with neutralizing tank；Neutralizing tank is connected with wastewater discharge pipe, alternatively,
Neutralizing tank is connect by delivery pipe with reclamation set.
In each delivery pipe according to actual needs, it is provided with control valve.
In the technical scheme, it is related to working principle are as follows:
In electrodialysis separation system, power supply positive and negative polarities directly replace, parallel placement anode membrane and cavity block, anode membrane and cavity block structure
Film forming group, and being spaced apart film group and film group with partition, form freshwater room and concentrated water room.Hemicellulose is passed through into freshwater room
Hydrolyzate material is passed through demineralized water into concentrated water room, under the action of DC electric field, in freshwater room cation (sodium ion, hydrogen from
Son) it is migrated to cathode, cation-exchange membrane can only be passed through；Anion (sulfate ion, hydroxide ion) is migrated to anode, only
It can be by anion-exchange membrane, so that sodium sulphate and sulfuric acid desalination in freshwater room；Sodium sulphate and sulfuric acid are concentrated in concentrated water room, will
High saline solution and high liquid glucose are drawn respectively, to reach desalination, depickling purpose.
The present invention is to fully ensure that electrodialysis effect, carries out first order electrodialysis, second level electrodialysis and third level electric osmose
Analyse operation；Since content of reducing sugar is 13~15g/L in the high saline solution of the third level and conductance is 20~30ms/cm, and the first order is high
Content of reducing sugar is 75~90g/L in liquid glucose and conductance is 40~50ms/cm, based on the ratio between reduced sugar and conductance
Speech, the sugared salt of the high saline solution of the third level is relatively low, and can prepare raw material directly as xylose after its concentration and desalination (de- conductance) makes
With, so, with the high liquid glucose of the third level together as meet index (conductance≤4000us/cm, refractive power >=7.0, inorganic acid≤
0.3%, total acid≤0.4%, content of reducing sugar >=70g/L, Xylose Content >=55g/L and xylose purity >=80%) final feed liquid into
Enter subsequent processing；It can direct emission or reuse after the high saline solution dilution of the first order, neutralization.
Using the technical program, bring advantageous effects are as follows:
One, the present invention is applied to desalination, the depickling of hemicellulose hydrolysate, and then reaches removal of impurities to xylose solution, purifying mesh
, under the premise of improving xylose quality and production efficiency, reduces and run sugar amount (70~80%), increase economic efficiency.Meanwhile subtracting
The discharge of few difficult sewage, is greatly improved environmental benefit, reduces environmental protection pressure, such as: reduce organic emission about 3.5
Ton/day, sewage disposal expense saves about 12 yuan/ton, and sewage load reduces 200 cubes/day etc.；
Two, the present invention removes electrolyte using electroosmose process, operating efficiency and the validity except electrolyte is improved, so that controllability is more
Height, and effectively avoid introducing new impurity, reduces cost, and by about 2.5 ten thousand yuan/day of profit increase；
Three, in the present invention, by after the high saline solution of the third level is concentrated and desalination, with the high liquid glucose of the third level together as meeting index
Final feed liquid enter subsequent processing, sugar amount will be run and reduced by 10% to 2~3%, and by about 2.8 ton/days of xylose output increased；
Four, it in the present invention, is largely recovered due to running sugar, the service life of electrodialysis plant increases considerably (the diaphragm longevity
Life improves 30% or more), this not only increases the stability of xylose preparation process, but also also improves equipment usability, reduces equipment
The cost of consumption.
Detailed description of the invention
Fig. 1 is the logic connectivity diagram of electrodialysis separation system in the present invention；
Fig. 2 is the workflow block diagram of electrodialysis separation system in the present invention；
Fig. 3 is the electrodialysis operation principle schematic diagram in the present invention；
Wherein, in figure: 1, desalination water storage tank, 2, first order electrodialysis plant, 3, second level electrodialysis plant, 4, third level electric osmose
Analysis apparatus, 5, delivery pipe, 6, temporary storage tank, 7, enrichment facility, 8, desalter, 9, thinning tank, 10, neutralizing tank, 11, ion exchange
Column.
Specific embodiment
Below by technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described reality
Applying example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without making creative work belongs to what the present invention protected
Range.
Embodiment 1
A kind of electrodialysis separating technology of hemicellulose hydrolysate, includes the following steps:
1) first order electrodialysis: hemicellulose hydrolysate is passed through to first order electrodialysis system, and is passed through the high saline solution in the second level,
It is acted on through electrodialytic membranes, obtains the high liquid glucose of the first order and the high saline solution of the first order；
2) second level electrodialysis: it will be passed through through the high liquid glucose of the resulting first order of step 1) to second level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high saline solution of the high liquid glucose in the second level and the second level；
3) third level electrodialysis: it will be passed through through the high liquid glucose in the resulting second level of step 2 to third level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high liquid glucose of the third level and the high saline solution of the third level；
4) it post-processes: after the high saline solution concentration of the third level and desalination, being stored in temporary storage tank together with the high liquid glucose of the third level, so
Afterwards, it is injected into ion exchange column, is chromatographed using the mature prior art, obtain xylose solution.
Embodiment 2
On the basis of embodiment 1, further:
The hemicellulose hydrolysate refers to: using hemicellulose as raw material, after sulphuric acid hydrolysis, being carried out using existing mature technology
Hemicellulose hydrolysate after the pre-treatments such as filtering, decoloration, ultrafiltration.Wherein, in the hemicellulose hydrolysate, Xylose Content
For 70~90g/L, 20~22g/L of sodium sulphate content, 20~25g/L of sulfuric acid content.
Embodiment 3
It is further on the basis of embodiment 2:
Further, in the first order electrodialysis system of step 1), hemicellulose hydrolysate feed rate is 40m3/ h, second
The high saline solution feed rate of grade is 15m3/h；Voltage is 150V, and electric current 100A, temperature is 40 DEG C；The high saline solution reactor effluent stream of the first order
Amount is 15m3/ h, the high liquid glucose discharging flow of the first order are 40m3/h；
In the second level electrodialysis system of step 2, the high liquid glucose feed rate of the first order is 40m3/ h, demineralized water feed rate
For 15m3/h；Voltage is 150V, and electric current 100A, temperature is 40 DEG C；The high saline solution discharging flow in the second level is 15m3/ h, the second level
High liquid glucose discharging flow is 40m3/h；
In the third level electrodialysis system of step 3), the high liquid glucose feed rate in the second level is 40m3/ h, demineralized water feed rate
For 15m3/h；Voltage is 150V, and electric current 75A, temperature is 40 DEG C；The high saline solution discharging flow of the third level is 15m3/ h, the third level are high
Liquid glucose discharging flow is 40m3/h。
Embodiment 4
On the basis of embodiment 3, the present embodiment difference is:
Further, in the first order electrodialysis system of step 1), hemicellulose hydrolysate feed rate is 50m3/ h, second
The high saline solution feed rate of grade is 17m3/h；Voltage is 150V, and electric current 100A, temperature is 45 DEG C；The high saline solution reactor effluent stream of the first order
Amount is 17m3/ h, the high liquid glucose discharging flow of the first order are 50m3/h；
In the second level electrodialysis system of step 2, the high liquid glucose feed rate of the first order is 50m3/ h, demineralized water feed rate
For 17m3/h；Voltage is 150V, and electric current 100A, temperature is 45 DEG C；The high saline solution discharging flow in the second level is 17m3/ h, the second level
High liquid glucose discharging flow is 50m3/h；
In the third level electrodialysis system of step 3), the high liquid glucose feed rate in the second level is 50m3/ h, demineralized water feed rate
For 17m3/h；Voltage is 150V, and electric current 100A, temperature is 45 DEG C；The high saline solution discharging flow of the third level is 17m3/ h, the third level
High liquid glucose discharging flow is 50m3/h。
Embodiment 5
On the basis of embodiment 3-4, the present embodiment difference is:
Further, in the first order electrodialysis system of step 1), hemicellulose hydrolysate feed rate is 45m3/ h, second
The high saline solution feed rate of grade is 16m3/h；Voltage is 150V, and electric current 100A, temperature is 42 DEG C；The high saline solution reactor effluent stream of the first order
Amount is 16m3/ h, the high liquid glucose discharging flow of the first order are 45m3/h；
In the second level electrodialysis system of step 2, the high liquid glucose feed rate of the first order is 45m3/ h, demineralized water feed rate
For 16m3/h；Voltage is 150V, and electric current 100A, temperature is 42 DEG C；The high saline solution discharging flow in the second level is 16m3/ h, the second level
High liquid glucose discharging flow is 45m3/h；
In the third level electrodialysis system of step 3), the high liquid glucose feed rate in the second level is 45m3/ h, demineralized water feed rate
For 16m3/h；Voltage is 150V, and electric current 86A, temperature is 42 DEG C；The high saline solution discharging flow of the third level is 16m3/ h, the third level are high
Liquid glucose discharging flow is 45m3/h。
Embodiment 6
It is further on the basis of embodiment 3-5:
In step 1), 2) and 3) in, the electrodialytic membranes is alloy film.
Embodiment 7
It is further on the basis of embodiment 6:
It in the enrichment process of step 4), is concentrated using homogeneous electrodialytic membranes, the high saline solution conductance of the third level after concentration is
200ms/cm。
In step 4) desalination process, desalination is carried out using alloy film, the high saline solution conductance of the third level after desalination is 5ms/
cm。
Embodiment 8
On the basis of embodiment 7, the present embodiment difference is:
It in the enrichment process of step 4), is concentrated using alloy film, the high saline solution conductance of the third level after concentration is 250 ms/
cm。
In step 4) desalination process, desalination is carried out using alloy film, the high saline solution conductance of the third level after desalination is 3ms/
cm。
Embodiment 9
On the basis of embodiment 7-8, the present embodiment difference is:
It in the enrichment process of step 4), is concentrated using homogeneous electrodialytic membranes, the high saline solution conductance of the third level after concentration is
230 ms/cm。
In step 4) desalination process, desalination is carried out using alloy film, the high saline solution conductance of the third level after desalination is 4 ms/
cm。
Embodiment 10
It is further on the basis of embodiment 7-9:
In step 1), the high saline solution of the first order include concentration be 17g/L reduced sugar, concentration is 35g/L sulfuric acid and concentration is 15g/L
Sodium sulphate；The high liquid glucose of the first order include concentration be 75g/L reduced sugar, concentration is 12g/L sulfuric acid and concentration is 5g/L sodium sulphate；
In step 2, the high saline solution in the second level include concentration be 15g/L reduced sugar, concentration is 20g/L sulfuric acid and concentration is 15g/L
Sodium sulphate；The high liquid glucose in the second level include concentration be 75g/L reduced sugar, concentration is 5g/L sulfuric acid and concentration is 5g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 13g/L reduced sugar, concentration is 5g/L sulfuric acid and concentration is 5g/L sulphur
Sour sodium；The high liquid glucose of the third level include concentration be 75g/L reduced sugar, concentration is 1g/L sulfuric acid and concentration is 1g/L sodium sulphate.
In step 1), the high saline solution conductance of the first order is 150ms/cm, pH 0.5, refractive power 5.5；The high liquid glucose of the first order
Conductance is 40ms/cm, pH 1.0, refractive power 8.0；
In step 2, the high saline solution conductance in the second level is 70ms/cm, pH 1.0, refractive power 3；The high liquid glucose conductance in the second level is
18ms/cm, pH 1.8, refractive power 8.0；
In step 3), the high saline solution conductance of the third level is 20ms/cm, pH 2, refractive power 1；The high liquid glucose conductance of the third level is 3ms/
Cm, pH 2.2, refractive power 8.0.
Embodiment 11
On the basis of embodiment 10, the present embodiment difference is:
In step 1), the high saline solution of the first order include concentration be 20g/L reduced sugar, concentration is 45g/L sulfuric acid and concentration is 18g/L
Sodium sulphate；The high liquid glucose of the first order include concentration be 90g/L reduced sugar, concentration is 14g/L sulfuric acid and concentration is 10g/L sodium sulphate；
In step 2, the high saline solution in the second level include concentration be 18g/L reduced sugar, concentration is 35g/L sulfuric acid and concentration is 18g/L
Sodium sulphate；The high liquid glucose in the second level include concentration be 90g/L reduced sugar, concentration is 10g/L sulfuric acid and concentration is 10g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 15g/L reduced sugar, concentration is 8g/L sulfuric acid and concentration is 5~8g/
L sodium sulphate；The high liquid glucose of the third level include concentration be 90g/L reduced sugar, concentration is 2g/L sulfuric acid and concentration is 2g/L sodium sulphate.
In step 1), the high saline solution conductance of the first order is 180ms/cm, pH 1.0, refractive power 6.5；The high liquid glucose of the first order
Conductance is 50ms/cm, pH 1.3, refractive power 9.0；
In step 2, the high saline solution conductance in the second level is 80ms/cm, pH 1.2, refractive power 4；The high liquid glucose conductance in the second level is
20ms/cm, pH 2.1, refractive power 9.0；
In step 3), the high saline solution conductance of the third level is 23ms/cm, pH 2.2, refractive power 2；The high liquid glucose conductance of the third level is
4ms/cm, pH 22.8, refractive power 9.0.
Embodiment 12
On the basis of embodiment 10-11, the present embodiment difference is:
In step 1), the high saline solution of the first order include concentration be 18g/L reduced sugar, concentration is 40g/L sulfuric acid and concentration is 16g/L
Sodium sulphate；The high liquid glucose of the first order include concentration be 85g/L reduced sugar, concentration is 13g/L sulfuric acid and concentration is 8g/L sodium sulphate；
In step 2, the high saline solution in the second level include concentration be 17g/L reduced sugar, concentration is 25g/L sulfuric acid and concentration is 16g/L
Sodium sulphate；The high liquid glucose in the second level include concentration be 85g/L reduced sugar, concentration is 7g/L sulfuric acid and concentration is 9g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 14g/L reduced sugar, concentration is 7g/L sulfuric acid and concentration is 6g/L sulphur
Sour sodium；The high liquid glucose of the third level include concentration be 85g/L reduced sugar, concentration is 1.5g/L sulfuric acid and concentration is 1.5g/L sodium sulphate.
In step 1), the high saline solution conductance of the first order is 165ms/cm, pH 0.8, refractive power 6.0；The high liquid glucose of the first order
Conductance is 45ms/cm, pH 1.1, refractive power 8.5；
In step 2, the high saline solution conductance in the second level is 75ms/cm, pH 1.1, refractive power 3.5；The high liquid glucose conductance in the second level is
19ms/cm, pH 2.0, refractive power 8.5；
In step 3), the high saline solution conductance of the third level is 25ms/cm, pH 2.1, refractive power 1.5；The high liquid glucose conductance of the third level is
3.5ms/cm, pH 2.6, refractive power 8.5.
Embodiment 13
A kind of electrodialysis separating technology of hemicellulose hydrolysate, includes the following steps:
1) first order electrodialysis: hemicellulose hydrolysate is passed through to first order electrodialysis system, and is passed through the high saline solution in the second level
(electrodialysis system is for the first time in use, be passed through demineralized water.When electrodialysis system operates normally, i.e., second level electrodialysis system produces
Raw discharging flow is 17m3The high saline solution in the second level of/h, stopping are passed through demineralized water, switch to be passed through the high saline solution in the second level), through electric osmose
Film effect is analysed, the high liquid glucose of the first order and the high saline solution of the first order are obtained；
Hemicellulose hydrolysate feed rate is 40m3/ h, the high saline solution feed rate in the second level are 17m3/h；Voltage is 150V, electricity
Stream is 100A, and temperature is 45 DEG C；The high saline solution discharging flow of the first order is 17m3/ h, the high liquid glucose discharging flow of the first order are 40m3/h；
2) second level electrodialysis: it will be passed through through the high liquid glucose of the resulting first order of step 1) to second level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high saline solution of the high liquid glucose in the second level and the second level；
The high liquid glucose feed rate of the first order is 40m3/ h, demineralized water feed rate are 17m3/h；Voltage is 150V, and electric current is
100A, temperature are 45 DEG C；The high saline solution discharging flow in the second level is 17m3/ h, the high liquid glucose discharging flow in the second level are 40m3/h；
3) third level electrodialysis: it will be passed through through the high liquid glucose in the resulting second level of step 2 to third level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high liquid glucose of the third level and the high saline solution of the third level；
The high liquid glucose feed rate in the second level is 40m3/ h, demineralized water feed rate are 17m3/h；Voltage is 150V, electric current 85A,
Temperature is 45 DEG C；The high saline solution discharging flow of the third level is 17m3/ h, the high liquid glucose discharging flow of the third level are 40m3/h。
4) it post-processes: after the high saline solution of the third level is carried out concentration and desalination, being stored in together with the high liquid glucose of the third level temporary
It in tank, then, is injected into ion exchange column, chromatographs, obtain xylose solution.
The hemicellulose hydrolysate refers to: with hemicellulosic material, after sulphuric acid hydrolysis, using existing mature technology into
Hemicellulose hydrolysate after the pre-treatments such as row filtering, decoloration, ultrafiltration.Wherein, in the hemicellulose hydrolysate, xylose contains
Amount is 85g/L, sodium sulphate content 21g/L, sulfuric acid content 23g/L.
In step 1), 2) and 3) in, the electrodialytic membranes is alloy film.
It in the enrichment process of step 4), is concentrated using alloy film, the high saline solution conductance of the third level after concentration is
220ms/cm。
In step 4) desalination process, desalination is carried out using alloy film, the high saline solution conductance of the third level after desalination is 4ms/
cm。
In step 1), the high saline solution of the first order include concentration be 20g/L reduced sugar, concentration is 35g/L sulfuric acid and concentration is
18g/L sodium sulphate；The high liquid glucose of the first order include concentration be 75g/L reduced sugar, concentration is 14g/L sulfuric acid and concentration is 5g/L sulfuric acid
Sodium；
In step 2, the high saline solution in the second level include concentration be 15g/L reduced sugar, concentration is 20g/L sulfuric acid and concentration is 18g/L
Sodium sulphate；The high liquid glucose in the second level include concentration be 75g/L reduced sugar, concentration is 10g/L sulfuric acid and concentration is 5g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 15g/L reduced sugar, concentration is 8g/L sulfuric acid and concentration is 5g/L sulphur
Sour sodium；The high liquid glucose of the third level include concentration be 75g/L reduced sugar, concentration is 2g/L sulfuric acid and concentration is 1g/L sodium sulphate.
According to standard " GB/T23532-2009 xylose ", through detecting, the hemicellulose hydrolysate is after electrodialysis separates:
Conductance≤4000us/cm, light transmittance >=98.0%, refractive power >=7.0,18.5 °~19.5 ° of specific rotatory power, pH is 2.2~2.8；Also
Raw sugar content >=70g/L, Xylose Content >=55g/L, xylose purity >=80%；Inorganic acid≤0.3%, total acid≤0.4%, sulfate
Content≤0.005%, ash content≤0.05%, moisture≤0.3%, chloride≤0.005%.
Embodiment 14
As shown in Figs. 1-3: electrodialysis separation system includes desalination water storage tank 1 and electrodialysis plant, and the electrodialysis plant is three
It is a, respectively first order electrodialysis plant 2, second level electrodialysis plant 3 and third level electrodialysis plant 4, first order electrodialysis
Device 2 is connect with second level electrodialysis plant 3, forms first between first order electrodialysis plant 2 and second level electrodialysis plant 3
Grade electrodialysis system；Second level electrodialysis plant 3 is connect with desalination water storage tank 1, desalination water storage tank 1 and second level electrodialysis plant
Second level electrodialysis system is formed between 3；Second level electrodialysis plant 3 is connect with third level electrodialysis plant 4, third level electric osmose
Analysis apparatus 4 is connect with desalination water storage tank 1, and third level electrodialysis system is formed between desalination water storage tank 1 and third level electrodialysis plant 4
System.
Further, 2 feed inlet of first order electrodialysis plant is connected with the delivery pipe 5 of conveying hemicellulose hydrolysate,
The outlet of the high liquid glucose of first order electrodialysis plant 2 is connect by delivery pipe 5 with 3 feed inlet of second level electrodialysis plant, second level electricity
The outlet of the high saline solution of electrodialysis apparatus 3 is connect by delivery pipe 5 with first order electrodialysis plant 2, the high liquid glucose of second level electrodialysis plant 3
Outlet is connect by delivery pipe 5 with 4 feed inlet of third level electrodialysis plant；The outlet of the high liquid glucose of third level electrodialysis plant 4 passes through
Delivery pipe 5 is connected with temporary storage tank 6, and the outlet of the high saline solution of third level electrodialysis plant 4 is connect by delivery pipe 5 with temporary storage tank 6.
Further, enrichment facility 7 is additionally provided between the outlet of the third level electrodialysis plant 4 high saline solution and temporary storage tank 6
With desalter 8, the outlet of the high saline solution of third level electrodialysis plant 4 is connect with enrichment facility 7, and enrichment facility 7 and desalter 8 connect
It connects, desalter 8 is connect with temporary storage tank 6, and temporary storage tank 6 is connected with ion exchange column 11.
Further, the electrodialysis separation system further includes thinning tank 9 II and neutralizing tank 10, first order electrodialysis plant
2 high saline solution outlets are connect by delivery pipe 5 with thinning tank 9 II, and thinning tank 9 II is connect with neutralizing tank 10；Neutralizing tank 10 is connected with
Wastewater discharge pipe, alternatively, neutralizing tank 10 is connect by delivery pipe 5 with reclamation set.
Embodiment 15
A kind of electrodialysis separating technology of hemicellulose hydrolysate, includes the following steps:
1) first order electrodialysis: hemicellulose hydrolysate is passed through to first order electrodialysis system, is passed through the high saline solution in the second level, warp
Electrodialytic membranes acts on (condition such as the following table 1), obtains the high liquid glucose of the first order and the high saline solution of the first order (such as following table 4-5)；
2) second level electrodialysis: it will be passed through through the high liquid glucose of the resulting first order of step 1) to second level electrodialysis system, and be passed through and remove
Salt water acts on (condition such as the following table 2) through electrodialytic membranes, obtains the high saline solution of the high liquid glucose in the second level and the second level (such as following table 4-5)；
3) third level electrodialysis: it will be passed through through the high liquid glucose in the resulting second level of step 2 to third level electrodialysis system, and be passed through and remove
Salt water acts on (condition such as the following table 3) through electrodialytic membranes, obtains the high liquid glucose of the third level and the high saline solution of the third level (such as following table 4-5)；
4) it post-processes: after the high saline solution of the third level is carried out concentration and desalination, being stored in temporary storage tank together with the high liquid glucose of the third level,
Then, it is injected into ion exchange column, chromatographs, obtain xylose solution.
Claims (10)
1. a kind of electrodialysis separating technology of hemicellulose hydrolysate, which comprises the steps of:
1) first order electrodialysis: hemicellulose hydrolysate is passed through to first order electrodialysis system, and is passed through the high saline solution in the second level,
It is acted on through electrodialytic membranes, obtains the high liquid glucose of the first order and the high saline solution of the first order；
2) second level electrodialysis: it will be passed through through the high liquid glucose of the resulting first order of step 1) to second level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high saline solution of the high liquid glucose in the second level and the second level；
3) third level electrodialysis: it will be passed through through the high liquid glucose in the resulting second level of step 2 to third level electrodialysis system, and be passed through
Demineralized water is acted on through electrodialytic membranes, obtains the high liquid glucose of the third level and the high saline solution of the third level；
4) it post-processes: after the high saline solution concentration of the third level and desalination, being stored in temporary storage tank together with the high liquid glucose of the third level, so
Afterwards, it is injected into ion exchange column, chromatographs, obtain xylose solution.
2. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that in step 1)
In, the hemicellulose hydrolysate include content be 70~90g/L xylose, content is 20~22g/L sodium sulphate and content is 20
~25g/L sulfuric acid.
3. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that in step 4)
In, the high saline solution conductance of the third level after concentration is 200~250 ms/cm；The high saline solution conductance of the third level after desalination is 3~5
ms/cm。
4. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that in step 1)
In first order electrodialysis system, hemicellulose hydrolysate feed rate is 40~50m3/ h, the high saline solution feed rate in the second level are
15~17m3/h；Voltage is 150V, and electric current 100A, temperature is 40~45 DEG C；The high saline solution discharging flow of the first order be 15~
17m3/ h, the high liquid glucose discharging flow of the first order are 40~50m3/h；
In the second level electrodialysis system of step 2, the high liquid glucose feed rate of the first order is 40~50m3/ h, demineralized water feeding flow
Amount is 15~17m3/h；Voltage is 150V, and electric current 100A, temperature is 40~45 DEG C；The high saline solution discharging flow in the second level is 15
~17m3/ h, the high liquid glucose discharging flow in the second level are 40~50m3/h；
In the third level electrodialysis system of step 3), the high liquid glucose feed rate in the second level is 40~50m3/ h, demineralized water feeding flow
Amount is 15~17m3/h；Voltage is 150V, and electric current is 75~100A, and temperature is 40~45 DEG C；The high saline solution discharging flow of the third level
For 15~17m3/ h, the high liquid glucose discharging flow of the third level are 40~50m3/h。
5. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that in step 1)
In, the high saline solution of the first order include concentration be 17~20g/L reduced sugar, concentration is 35~45g/L sulfuric acid and concentration is 15~18g/L
Sodium sulphate；The high liquid glucose of the first order include concentration be 75~90g/L reduced sugar, concentration is 12~14g/L sulfuric acid and concentration be 5~
10g/L sodium sulphate；
In step 2, the high saline solution in the second level include concentration be 15~18g/L reduced sugar, concentration is 20~35g/L sulfuric acid and dense
Degree is 15~18g/L sodium sulphate；The high liquid glucose in the second level include concentration be 75~90g/L reduced sugar, concentration is 5~10g/L sulfuric acid
And concentration is 5~10g/L sodium sulphate；
In step 3), the high saline solution of the third level include concentration be 13~15g/L reduced sugar, concentration is 5~8g/L sulfuric acid and concentration
For 5~8g/L sodium sulphate；The high liquid glucose of the third level include concentration be 75~90g/L reduced sugar, concentration is 1~2g/L sulfuric acid and concentration
For 1~2g/L sodium sulphate.
6. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that in step 1)
In, the high saline solution conductance of the first order is 150~180ms/cm, and pH is 0.5~1.0, and refractive power is 5.5~6.5；The high liquid glucose electricity of the first order
Leading as 40~50ms/cm, pH is 1.0~1.3, and refractive power is 8.0~9.0；
In step 2, the high saline solution conductance in the second level is 70~80ms/cm, and pH is 1.0~1.2, and refractive power is 3~4；The second level is high
Liquid glucose conductance is 18~20ms/cm, and pH is 1.8~2.1, and refractive power is 8.0~9.0；
In step 3), the high saline solution conductance of the third level is 20~30ms/cm, and pH is 2~2.2, and refractive power is 1~2；The high sugar of the third level
Liquid conductance is 3~4ms/cm, and pH is 2.2~2.8, and refractive power is 8.0~9.0.
7. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that through electrodialysis point
From rear, detection feed liquid is simultaneously obtained: conductance≤4000us/cm, light transmittance >=98.0%, refractive power >=7.0,18.5 ° of specific rotatory power~
19.5 °, pH is 2.2~2.8；Content of reducing sugar >=70g/L, Xylose Content >=55g/L, xylose purity >=80%；Inorganic acid≤
0.3%, total acid≤0.4%, sulphates content≤0.005%, ash content≤0.05%, moisture≤0.3%, chloride≤0.005%.
8. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 1, which is characterized in that carry out electrodialysis
Separating technology, involved electrodialysis separation system include desalination water storage tank (1) and electrodialysis plant, and the electrodialysis plant is three
It is a, respectively first order electrodialysis plant (2), second level electrodialysis plant (3) and third level electrodialysis plant (4), the first order
Electrodialysis plant (2) is connect with second level electrodialysis plant (3), first order electrodialysis plant (2) and second level electrodialysis plant
(3) first order electrodialysis system is formed between；Second level electrodialysis plant (3) is connect with desalination water storage tank (1), desalination water storage tank
(1) second level electrodialysis system is formed between second level electrodialysis plant (3)；Second level electrodialysis plant (3) and the third level
Electrodialysis plant (4) connection, third level electrodialysis plant (4) are connect with desalination water storage tank (1), desalination water storage tank (1) and third
Third level electrodialysis system is formed between grade electrodialysis plant (4).
9. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 8, which is characterized in that the first order
Electrodialysis plant (2) feed inlet is connected with the delivery pipe (5) of conveying hemicellulose hydrolysate, the high sugar of first order electrodialysis plant (2)
Liquid outlet is connect by delivery pipe (5) with second level electrodialysis plant (3) feed inlet, second level electrodialysis plant (3) high saline solution
Outlet is connect by delivery pipe (5) with first order electrodialysis plant (2), and the high liquid glucose outlet of second level electrodialysis plant (3) passes through
Delivery pipe (5) is connect with third level electrodialysis plant (4) feed inlet；The high liquid glucose outlet of third level electrodialysis plant (4) passes through defeated
Pipe (5) is sent to be connected with temporary storage tank (6), the high saline solution outlet of third level electrodialysis plant (4) passes through delivery pipe (5) and temporary storage tank (6)
Connection.
10. the electrodialysis separating technology of hemicellulose hydrolysate according to claim 9, which is characterized in that the third
Enrichment facility (7) and desalter (8), the third level are additionally provided between the high saline solution outlet of grade electrodialysis plant (4) and temporary storage tank (6)
The high saline solution outlet of electrodialysis plant (4) is connect with enrichment facility (7), and enrichment facility (7) is connect with desalter (8), desalination dress
It sets (8) to connect with temporary storage tank (6), temporary storage tank (6) is connected with ion exchange column (11).
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