CN107475466A - The technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose - Google Patents
The technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose Download PDFInfo
- Publication number
- CN107475466A CN107475466A CN201710773954.XA CN201710773954A CN107475466A CN 107475466 A CN107475466 A CN 107475466A CN 201710773954 A CN201710773954 A CN 201710773954A CN 107475466 A CN107475466 A CN 107475466A
- Authority
- CN
- China
- Prior art keywords
- ozone
- hemicellulose
- xylose
- pipe
- technique
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Organic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to the technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose, belong to xylose preparing technical field.The present invention is handled with ozone, pass through specific aeration mode, reach the limited oxidation to hemicellulose, it is set finally to be reacted with hemicellulose into carbon dioxide and water, and the chemical bond partial destruction in hemicellulose can only be created conditions for sour water solution, therefore sour water solution can is used in the environment of relatively low temperature, the production of reaction target product five-carbon ring aldehydo sugar product is realized, improves yield.The technique uses ozone and sour hydrolysis process hemicellulose, can shorten sour hydrolysis time, and environment friendly and pollution-free.
Description
Technical field
The present invention relates to a kind of technique that xylose is prepared using hemicellulose, it is more particularly related to a kind of smelly
Oxygen acid hydrolyzed hemicellulose prepares the technique of xylose, belongs to xylose preparing technical field.
Background technology
Xylose is a component of xylan, and xylan is widely present in plant.Xylose exists in animal heparin, soft
In ossein and glycoprotein, it is sugar chain and serine in some glycoprotein（Or threonine）Connection unit, in nature so far
The xylose of free state is not found also.Xylose can be made in solution containing hemicellulose.
State Intellectual Property Office discloses a Publication No. CN102643935A, a kind of entitled " profit in 2012.8.22
The invention of the method for preparing xylose with spent lye is squeezed in production process of viscose fiber ", the invention are related to a kind of fine using viscose glue
The method that squeezing spent lye prepares xylose in dimension production process.The present invention passes through the preparation of hemicellulose solution, hemicellulose
Extraction, the hydrolysis of hemicellulose, neutralize depickling, pre-concentration, decolouring, ion exchange and Conventional concentration, crystallization, separation, drying
Process obtains xylose finished product.Using technical solution of the present invention, caused salkali waste, waste water in viscose glue production process can have been utterly destroyed
Deng the harmful substance of pollution environment, the standard of whole process clean manufacturing is can reach, makes viscose glue manufacturing enterprise in the same of production viscose glue
When, xylose can be also produced simultaneously, also accomplished refuse reclamation while reaching environmentally friendly purpose.
State Intellectual Property Office discloses a Publication No. CN101649570A, a kind of entitled " wheat in 2010.2.17
Wheat straw is placed in ethanol water by the invention of the low stain preparation technology of grass fiber element ", the invention, is dissolved under high temperature in wheat straw
Most of lignin and hemicellulose, be then dispersed in again in water, add MgSO4, and it is passed through oxygen in a heated condition
Filtered after further removing lignin and part hemicellulose and coarse product of cellulose is washed, then be passed through the remaining wood of ozone removing
Element and hemicellulose obtain cellulose products；Finally, filter and wash cellulose products, it is 8~12 to add alkali regulation pH value, and is added
Enter H2O2, heat, refilter, wash cellulose products pure after obtaining refining.The present invention uses low stain ethanol
Method decomposes wheat straw raw material, using oxygen, ozone, H2O2The technique of subsequent treatment is carried out in wheat straw etc. pollution-free chemical reagent
Cellulose is separated and refined, and has both been alleviated the problem in short supply of the conventional cellulose resource such as timber, cotton, has been taken full advantage of again
Agricultural wastes wheat straw resource.
Prior art hemicellulose solution acid hydrolysis time is grown, and xylose loss is big, and xylose yield is low.The effect handled with ozone
Fruit is bad, it is impossible to produces effecting reaction with liquid.
The content of the invention
Present invention seek to address that sour hydrolyzed hemicellulose prepares sour hydrolysis time length, xylose loss in xylose in the prior art
Greatly, a kind of the problem of xylose yield is low, there is provided the technique that ozone acid hydrolyzed hemicellulose prepares xylose.The technique using ozone and
Sour hydrolysis process hemicellulose, sour hydrolysis time can be shortened, xylose yield improves, and environment friendly and pollution-free.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
The technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose, it is characterised in that：Comprise the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes, every loading pipe
Top is both provided with exhaust gas collecting pipe, and material liquid inlet tube, the material liquid entrance are provided with above the exhaust gas collecting pipe
Pipe is connected by pipeline with the top of loading pipe every described；The hemicellulose solution passes through described in the inflow of material liquid inlet tube
In loading pipe；
B, ozone inlet pipe is provided with below the bottom of the loading pipe, be provided with the ozone inlet pipe it is multiple with it is described
The corresponding ozone nozzle of loading pipe, ozone enter from the ozone inlet pipe, are then sprayed into the loading pipe, to hemicellulose
Plain solution is handled, and hemicellulose solution converges to material liquid and collected in kettle after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle by ozone processing enters in hydrolysis case, to the hydrolysis
Acid is added in reaction chamber, is heated using steam, acid hydrolytic reaction is carried out, xylose and mixture is obtained after reaction；
D, xylose and mixture enter xylose separator；Ozone tail gas in the exhaust gas collecting pipe converges to the xylose point
From in device, the xylose and mixture are handled, then isolated primary xylose product.
Currently preferred, in step, the hemicellulose level of the hemicellulose solution containing hemicellulose is
5-7%。
Currently preferred, in step, the filler in the loading pipe is ceramic corrugated filler.
Currently preferred, in stepb, the concentration of the ozone is 10-20 mg/litres.
Currently preferred, in stepb, the ventilation intensity handled hemicellulose solution is 5-10m3/
h。
Currently preferred, in step C, the concentration of the sulfuric acid is 1-2%.
Currently preferred, in step C, the reaction temperature control of the acid hydrolytic reaction is 60-80 DEG C, the reaction time
For below 1h.
Currently preferred, in step D, the concentration of the ozone is 4-9 mg/litres.
The advantageous effects that the present invention is brought：
1st, the present invention solves sour hydrolyzed hemicellulose in the prior art and prepares sour hydrolysis time length in xylose, and xylose loss is big,
A kind of the problem of xylose yield is low, there is provided the technique that ozone acid hydrolyzed hemicellulose prepares xylose.The technique uses ozone and acid
Hydrolysis process hemicellulose, sour hydrolysis time can be shortened, xylose yield improves, and environment friendly and pollution-free.
2nd, the present invention is handled with ozone, by specific aeration mode, is reached the limited oxidation to hemicellulose, is made it most
It can not be reacted eventually with hemicellulose into carbon dioxide and water, and can only be sour water by the chemical bond partial destruction in hemicellulose
Solution is created conditions, therefore sour water solution can is used in the environment of relatively low temperature, realizes reaction target product five-carbon ring aldehydo sugar
The production of product, improve yield.
3rd, the present invention is handled with ozone, on the basis of by specific aeration mode, the concentration of further control ozone,
Aeration quantity, acid hydrolytic reaction can be more conducive to, further improves yield.
4th, the present invention carries out an ozone processing by each before and after sour water solution, reaches sterilization and decomposes hemicellulose Cheng little Fen
The purpose of son, be advantageous to hemicellulose and hydrolyzed in acid hydrolysis process more fully, shorten sour hydrolysis time, reduce high-temperature acid hydrolysis
Excessively cause xylose to lose, increase xylose yield, reducing reaction needs temperature, so as to save the energy.
5th, product xylose of the invention is five-carbon ring aldehydo sugar, and ozone usage is excessive, can cause xylose resolve into carbon dioxide and
Water, therefore, multitube aeration of the present invention reach uniform, control the concentration and aeration quantity of ozone（Ventilation intensity）, reach preferable place
Manage effect.
6th, the present invention has carried out an ozone processing again after an acidic hydrolysis, carries out disinfection, and further hydrolysis acid decomposes endless
Full hemicellulose, improve xylose yield.Preferable further control ozone concentration and ventilation intensity, improve treatment effect.It is smelly
Oxygen itself is nontoxic, pollution-free, remaining ozone, finally also synthesizes oxygen naturally, good to environmental protection.
7th, given in sour water solution of the invention, control specific acid concentration, avoid damage to xylose, prevent from excessively hydrolyzing xylose
Chemical bond rupture and degrade.
Brief description of the drawings
Fig. 1 is the structural representation for the equipment that present invention process uses；
Fig. 2 is exhaust gas collecting pipe structural representation in the equipment that present invention process uses；
Fig. 3 is ozone nozzle arrangements schematic diagram in the equipment that present invention process uses.
Reference：1 it is aerator, 2 be hydrolysis case, 3 be xylose separator, 4 be loading pipe, 5 is ozone
Inlet tube, 6 be exhaust gas collecting pipe, 7 be material liquid inlet tube, 8 be ozone nozzle, 9 be material liquid collect kettle, 10 be xylose mixing
Thing outlet, 11 be card, 12 be sour entrance, 13 be steam inlet, 14 be condensation-water drain, 15 be steam pipe, 16 be that tail gas goes out
Mouthful, 17 be that xylose exports, 18 is demister support frame, 19 is umbrella demister, 20 is nozzle body, 21 is nozzle cover, 22 is
Tapered portion, 23 be cylindrical portion, 24 be conical nozzle, 25 be ozone spout.
Embodiment
Embodiment 1
A kind of ozone acid hydrolyzed hemicellulose prepares the technique of xylose, comprises the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes 4, the every loading pipe 4
Top be both provided with exhaust gas collecting pipe 6, the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid
Inlet tube 7 is connected by pipeline with the top of loading pipe every described 4；The hemicellulose solution passes through material liquid inlet tube 7
Flow into the loading pipe 4；
B, ozone inlet pipe 5 is provided with below the bottom of the loading pipe 4, be provided with the ozone inlet pipe 5 it is multiple with
The corresponding ozone nozzle 8 of the loading pipe 4, ozone enter from the ozone inlet pipe 5, are then sprayed into the loading pipe 4,
Hemicellulose solution is handled, hemicellulose solution converges to material liquid and collected in kettle 9 after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle 9 by ozone processing enters in hydrolysis case 2, to the water
Solve and acid is added in reaction chamber 2, heated using steam, carry out acid hydrolytic reaction, xylose and mixture are obtained after reaction；
D, xylose and mixture enter xylose separator 3；Ozone tail gas in the exhaust gas collecting pipe 6 converges to the xylose
In separator 3, the xylose and mixture are handled, then isolated primary xylose product.
Present invention increase ozone oxidation pretreatment so that hemicellulose long-chain is broken, cellulose oxidation, is advantageous in next step
Master operation acid hydrolysis process；By the hemicellulose of pretreatment（Containing a small amount of cellulose）When reaching xylose product, temperature, reaction when
Between reduce.
Routine prepares xylose process：Hemicellulose concentration 5-7% solution, the concentration of sulfuric acid 2%, 100-102 DEG C of temperature, reaction
Hour time 1-2.
Using technique of the invention after ozone：Hemicellulose concentration 5-7% solution, the concentration of sulfuric acid 2%, 60-80 DEG C of temperature,
Reaction time was reduced within 1 hour.Hemicellulose, which is fully hydrolyzed, obtains xylose and mixture.
Embodiment 2
The equipment that a kind of ozone acid hydrolyzed hemicellulose prepares xylose, including aerator 1, hydrolysis case 2 and xylose separation
Device 3；The aerator 1 includes more vertically disposed loading pipes 4 and ozone inlet pipe 5, the top of the every loading pipe 4
Portion is both provided with exhaust gas collecting pipe 6, and the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid entrance
Pipe 7 is connected by more pipelines with the top of loading pipe every described 4, is provided with below the bottom of the loading pipe 4 described
Ozone inlet pipe 5, multiple ozone nozzles 8 corresponding with the loading pipe 4 are provided with the ozone inlet pipe 5；It is described to fill out
The lower section connection material liquid of expects pipe 4 collects kettle 9, and the bottom that the material liquid collects kettle 9 connects the hydrolysis case 2, described
Wood sugar mixtures outlet 10 is provided with hydrolysis case 2, the wood sugar mixtures outlet 10 passes through xylose described in pipeline communication
Separator 3；The top of the exhaust gas collecting pipe 6 passes through xylose separator 3 described in pipeline communication.
Preferably, the loading pipe 4 is 50-70 roots.
It is preferable or further, a diameter of 50-100mm of the loading pipe 4.
Preferably, the material liquid inlet tube 7 and the ozone inlet pipe 5 are all horizontally disposed.
Preferably, the loading pipe 4 is by collecting the card 11 at the top of kettle 9 and the material liquid installed in the material liquid
Collect kettle 9 to connect, the ozone inlet pipe 5 stretches into the material liquid and collects kettle 9, each described ozone nozzle 8 and one
It is corresponding at the bottom opening of the loading pipe 4.
Preferably, the top of the hydrolysis case 2 is provided with sour entrance 12, and top is provided with steam inlet 13, bottom
Condensation-water drain 14 is provided with, the steam inlet 13 and the condensation-water drain 14 are by being arranged in the hydrolysis case
The steam pipe 15 in portion connects.
Preferably, the top of the xylose separator 3 is provided with offgas outlet 16, and bottom is provided with xylose outlet 17.
Preferably, it is provided with the umbrella demister 19 on demister support frame 18 in the exhaust gas collecting pipe 6.
Preferably, the ozone nozzle 8 includes nozzle body 20 and nozzle cover 21；The nozzle body 20 includes bottom
Tapered portion 22 and the cylindrical portion on top 23, interior big outer small conical nozzle 24 is provided with the side wall of the cylindrical portion 23；The spray
Mouth lid 21 covers the cylindrical portion 23, and the ozone spout 25 of tubulose is provided with the side wall of nozzle cover 21.Said structure can be prevented
Only liquid directly pours into ozone nozzle 8, prevents foreign matters from being blocked, and by the scattered injection of gas, increase gas film behavior connects with increase gas-liquid
Contacting surface is accumulated.
Further, the conical nozzle 24 and the ozone spout 25 are all horizontally disposed.
This equipment can carry out limited oxidation to hemicellulose, reaction generation carbon dioxide and water be avoided, only by hemicellulose
Chemical bond partial destruction in element, for the condition of sour water solution creation advantageously so that sour water solution can be at a lower temperature
Carry out, improve target product xylose（Pentose）Yield.
The reaction of gas and liquid is spread in a liquid by gas, mass transfer reaches effecting reaction.This equipment uses multitube
The reaction of road separate gas and liquid, gas is avoided when passing through liquid, gas can not reach effective directly through liquid
The purpose of reaction.
The loading pipe of this equipment reacts elementary cell as ozone oxidation hemicellulose, reaches and fully expands in half fibrinolytic liquid
Dissipate, mass transfer, make hemicellulose oxidation reaction abundant.
This equipment divides oxidized portion, sour hydrolyzable moiety and separate section, and equipment integration, reduction leakage, occupation of land are smaller.
This equipment can avoid Large Copacity, the caused formation for being vortexed, destroying stable air film and liquid film of large area aeration,
So as to cause the unstable of chemical reaction.
This equipment is preferable, and the loading pipe is 50-70 roots.The quantity of loading pipe directly affects the size of equipment, above-mentioned
Quantity can guaranteed efficiency, do not interfere with installation again.
The ozone nozzle of this equipment corresponds with loading pipe, after forming big fluid segmentation, the optimization of subenvironment, therefore,
Single tube diameter is preferred in 50-100mm, too it is small can cause pipeline convection current resistance it is excessive, cause the operability of equipment, be more than
Then pipeline is deteriorated 100mm to the segmentation effect of big fluid, therefore influences the oxidation of hemicellulose.
This equipment is preferable, and the loading pipe is by collecting card and the raw material at the top of kettle installed in the material liquid
Liquid collects kettle connection, and the ozone inlet pipe stretches into the material liquid and collects kettle, each described ozone nozzle and an institute
State corresponding at the bottom opening of loading pipe.Above-mentioned preferred scheme can ensure the scattered of the ozone gas of aeration, be formed a large amount of micro-
The air film of sight, reactive gas liquid reaction film is formed with liquid contact surface.
This equipment is preferable, and sour entrance is provided with the top of the hydrolysis case, and top is provided with steam inlet, bottom
It is provided with condensation-water drain, the steam inlet and the condensation-water drain and passes through the steaming that is arranged on inside the hydrolysis case
Steam pipe connects.Said structure can keep and control the solution concentration of acidification reaction.
This equipment is preferable, and the ozone nozzle includes nozzle body and nozzle cover；The nozzle body includes bottom
Tapered portion and the cylindrical portion on top, interior big outer small conical nozzle is provided with the side wall of the cylindrical portion；The nozzle cover covers
The cylindrical portion, the ozone spout of tubulose is provided with the nozzle cap sidewall.Above-mentioned preferred scheme can prevent liquid from directly filling
Enter fumarole, prevent foreign matters from being blocked, by the scattered injection of gas, increase gas film behavior and increase gas liquid interfacial area.
Embodiment 3
A kind of ozone acid hydrolyzed hemicellulose prepares the technique of xylose, comprises the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes 4, the every loading pipe 4
Top be both provided with exhaust gas collecting pipe 6, the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid
Inlet tube 7 is connected by pipeline with the top of loading pipe every described 4；The hemicellulose solution passes through material liquid inlet tube 7
Flow into the loading pipe 4；
B, ozone inlet pipe 5 is provided with below the bottom of the loading pipe 4, be provided with the ozone inlet pipe 5 it is multiple with
The corresponding ozone nozzle 8 of the loading pipe 4, ozone enter from the ozone inlet pipe 5, are then sprayed into the loading pipe 4,
Hemicellulose solution is handled, hemicellulose solution converges to material liquid and collected in kettle 9 after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle 9 by ozone processing enters in hydrolysis case 2, to the water
Solve and acid is added in reaction chamber 2, heated using steam, carry out acid hydrolytic reaction, xylose and mixture are obtained after reaction；
D, xylose and mixture enter xylose separator 3；Ozone tail gas in the exhaust gas collecting pipe 6 converges to the xylose
In separator 3, the xylose and mixture are handled, then isolated primary xylose product.
In step, the hemicellulose level of the hemicellulose solution containing hemicellulose is 5%.
In step, the filler in the loading pipe is ceramic corrugated filler.
In stepb, the concentration of the ozone is 10 mg/litres.
In stepb, the ventilation intensity handled hemicellulose solution is 5m3/h。
In step C, the concentration of the sulfuric acid is 1%.
In step C, the reaction temperature control of the acid hydrolytic reaction is 60 DEG C, reaction time 40min.
In step D, the concentration of the ozone is 4 mg/litres.
Embodiment 4
A kind of ozone acid hydrolyzed hemicellulose prepares the technique of xylose, comprises the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes 4, the every loading pipe 4
Top be both provided with exhaust gas collecting pipe 6, the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid
Inlet tube 7 is connected by pipeline with the top of loading pipe every described 4；The hemicellulose solution passes through material liquid inlet tube 7
Flow into the loading pipe 4；
B, ozone inlet pipe 5 is provided with below the bottom of the loading pipe 4, be provided with the ozone inlet pipe 5 it is multiple with
The corresponding ozone nozzle 8 of the loading pipe 4, ozone enter from the ozone inlet pipe 5, are then sprayed into the loading pipe 4,
Hemicellulose solution is handled, hemicellulose solution converges to material liquid and collected in kettle 9 after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle 9 by ozone processing enters in hydrolysis case 2, to the water
Solve and acid is added in reaction chamber 2, heated using steam, carry out acid hydrolytic reaction, xylose and mixture are obtained after reaction；
D, xylose and mixture enter xylose separator 3；Ozone tail gas in the exhaust gas collecting pipe 6 converges to the xylose
In separator 3, the xylose and mixture are handled, then isolated primary xylose product.
In step, the hemicellulose level of the hemicellulose solution containing hemicellulose is 7%.
In step, the filler in the loading pipe is ceramic corrugated filler.
In stepb, the concentration of the ozone is 20 mg/litres.
In stepb, the ventilation intensity handled hemicellulose solution is 10m3/h。
In step C, the concentration of the sulfuric acid is 2%.
In step C, the reaction temperature control of the acid hydrolytic reaction is 80 DEG C, reaction time 55min.
In step D, the concentration of the ozone is 9 mg/litres.
Embodiment 5
A kind of ozone acid hydrolyzed hemicellulose prepares the technique of xylose, comprises the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes 4, the every loading pipe 4
Top be both provided with exhaust gas collecting pipe 6, the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid
Inlet tube 7 is connected by pipeline with the top of loading pipe every described 4；The hemicellulose solution passes through material liquid inlet tube 7
Flow into the loading pipe 4；
B, ozone inlet pipe 5 is provided with below the bottom of the loading pipe 4, be provided with the ozone inlet pipe 5 it is multiple with
The corresponding ozone nozzle 8 of the loading pipe 4, ozone enter from the ozone inlet pipe 5, are then sprayed into the loading pipe 4,
Hemicellulose solution is handled, hemicellulose solution converges to material liquid and collected in kettle 9 after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle 9 by ozone processing enters in hydrolysis case 2, to the water
Solve and acid is added in reaction chamber 2, heated using steam, carry out acid hydrolytic reaction, xylose and mixture are obtained after reaction；
D, xylose and mixture enter xylose separator 3；Ozone tail gas in the exhaust gas collecting pipe 6 converges to the xylose
In separator 3, the xylose and mixture are handled, then isolated primary xylose product.
In step, the hemicellulose level of the hemicellulose solution containing hemicellulose is 6%.
In step, the filler in the loading pipe is ceramic corrugated filler.
In stepb, the concentration of the ozone is 15 mg/litres.
In stepb, the ventilation intensity handled hemicellulose solution is 7.5m3/h。
In step C, the concentration of the sulfuric acid is 1.5%.
In step C, the reaction temperature control of the acid hydrolytic reaction is 70 DEG C, reaction time 47min.
In step D, the concentration of the ozone is 6.5 mg/litres.
Embodiment 6
A kind of ozone acid hydrolyzed hemicellulose prepares the technique of xylose, comprises the following steps that：
A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes 4, the every loading pipe 4
Top be both provided with exhaust gas collecting pipe 6, the top of the exhaust gas collecting pipe 6 is provided with material liquid inlet tube 7, the material liquid
Inlet tube 7 is connected by pipeline with the top of loading pipe every described 4；The hemicellulose solution passes through material liquid inlet tube 7
Flow into the loading pipe 4；
B, ozone inlet pipe 5 is provided with below the bottom of the loading pipe 4, be provided with the ozone inlet pipe 5 it is multiple with
The corresponding ozone nozzle 8 of the loading pipe 4, ozone enter from the ozone inlet pipe 5, are then sprayed into the loading pipe 4,
Hemicellulose solution is handled, hemicellulose solution converges to material liquid and collected in kettle 9 after treatment；
C, the hemicellulose solution that the material liquid is collected in kettle 9 by ozone processing enters in hydrolysis case 2, to the water
Solve and acid is added in reaction chamber 2, heated using steam, carry out acid hydrolytic reaction, xylose and mixture are obtained after reaction；
D, xylose and mixture enter xylose separator 3；Ozone tail gas in the exhaust gas collecting pipe 6 converges to the xylose
In separator 3, the xylose and mixture are handled, then isolated primary xylose product.
In step, the hemicellulose level of the hemicellulose solution containing hemicellulose is 6.5%.
In step, the filler in the loading pipe is ceramic corrugated filler.
In stepb, the concentration of the ozone is 12 mg/litres.
In stepb, the ventilation intensity handled hemicellulose solution is 6m3/h。
In step C, the concentration of the sulfuric acid is 1.3%.
In step C, the reaction temperature control of the acid hydrolytic reaction is 66 DEG C, reaction time 45min.
In step D, the concentration of the ozone is 8 mg/litres.
Claims (8)
- A kind of 1. technique that ozone acid hydrolyzed hemicellulose prepares xylose, it is characterised in that：Comprise the following steps that：A, the hemicellulose solution containing hemicellulose is added to more vertically disposed loading pipes, every loading pipe Top is both provided with exhaust gas collecting pipe, and material liquid inlet tube, the material liquid entrance are provided with above the exhaust gas collecting pipe Pipe is connected by pipeline with the top of loading pipe every described；The hemicellulose solution passes through described in the inflow of material liquid inlet tube In loading pipe；B, ozone inlet pipe is provided with below the bottom of the loading pipe, be provided with the ozone inlet pipe it is multiple with it is described The corresponding ozone nozzle of loading pipe, ozone enter from the ozone inlet pipe, are then sprayed into the loading pipe, to hemicellulose Plain solution is handled, and hemicellulose solution converges to material liquid and collected in kettle after treatment；C, the hemicellulose solution that the material liquid is collected in kettle by ozone processing enters in hydrolysis case, to the hydrolysis Acid is added in reaction chamber, is heated using steam, acid hydrolytic reaction is carried out, xylose and mixture is obtained after reaction；D, xylose and mixture enter xylose separator；Ozone tail gas in the exhaust gas collecting pipe converges to the xylose point From in device, the xylose and mixture are handled, then isolated primary xylose product.
- 2. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 prepares xylose, it is characterised in that：In step In rapid A, the hemicellulose level of the hemicellulose solution containing hemicellulose is 5-7%.
- 3. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 prepares xylose, it is characterised in that：In step In rapid A, the filler in the loading pipe is ceramic corrugated filler.
- 4. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 prepares xylose, it is characterised in that：In step In rapid B, the concentration of the ozone is 10-20 mg/litres.
- 5. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 or 4 prepares xylose, it is characterised in that： In stepb, the ventilation intensity handled hemicellulose solution is 5-10m3/h。
- 6. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 prepares xylose, it is characterised in that：In step In rapid C, the concentration of the sulfuric acid is 1-2%.
- 7. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 or 6 prepares xylose, it is characterised in that： In step C, the reaction temperature control of the acid hydrolytic reaction is 60-80 DEG C, and the reaction time is below 1h.
- 8. the technique that a kind of ozone acid hydrolyzed hemicellulose according to claim 1 prepares xylose, it is characterised in that：In step In rapid D, the concentration of the ozone is 4-9 mg/litres.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710773954.XA CN107475466B (en) | 2017-08-31 | 2017-08-31 | Process for preparing xylose by hydrolyzing hemicellulose with ozone acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710773954.XA CN107475466B (en) | 2017-08-31 | 2017-08-31 | Process for preparing xylose by hydrolyzing hemicellulose with ozone acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107475466A true CN107475466A (en) | 2017-12-15 |
| CN107475466B CN107475466B (en) | 2020-12-04 |
Family
ID=60603200
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710773954.XA Active CN107475466B (en) | 2017-08-31 | 2017-08-31 | Process for preparing xylose by hydrolyzing hemicellulose with ozone acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107475466B (en) |
Citations (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62281890A (en) * | 1986-05-29 | 1987-12-07 | Norin Suisansyo Ringyo Shikenjo | Production of xylose and xylooligosaccharide |
| CN201136844Y (en) * | 2007-12-07 | 2008-10-22 | 山东福田药业有限公司 | Neutralization device for hydrolysate in production of xylose |
| CN101649570A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing wheatgrass cellulose with low pollution |
| CN101787398A (en) * | 2010-01-22 | 2010-07-28 | 中国科学院过程工程研究所 | Method for purifying, reclaiming and condensing sugar in lignocellulose prehydrolysis liquid |
| CN101962213A (en) * | 2010-10-21 | 2011-02-02 | 东南大学 | Energy-saving multitube photochemical excitation/oxidation water advanced treatment device |
| CN102643935A (en) * | 2012-04-11 | 2012-08-22 | 宜宾丝丽雅股份有限公司 | Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process |
| CN102899426A (en) * | 2012-10-25 | 2013-01-30 | 浙江华康药业股份有限公司 | Method for preparing xylose by using dissolving pulp wood chip prehydrolysis liquid |
| CN103074790A (en) * | 2012-12-25 | 2013-05-01 | 济南圣泉集团股份有限公司 | Comprehensive utilization process of biomass raw material |
| CN103193896A (en) * | 2013-03-12 | 2013-07-10 | 武汉纤浓生物科技有限公司 | Method of preparing konjac glucomannan and thin film evaporator used therein |
| CN103898246A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Method for producing xylose by using biomass raw material |
| CN103898247A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Technology for producing xylose from biomass raw materials |
| CN104109722A (en) * | 2014-07-01 | 2014-10-22 | 丽水学院 | Preparation method for xylo-oligosaccharide |
| CN104404108A (en) * | 2014-12-09 | 2015-03-11 | 齐鲁工业大学 | Pre-treating method for improving sugar conversion rate of lignocellulose |
| CN204752442U (en) * | 2015-06-26 | 2015-11-11 | 青岛科技大学 | Catalysis ozone oxidation promoters |
| CN105060458A (en) * | 2015-07-21 | 2015-11-18 | 黑龙江大学 | Water-purification device by utilizing catalytic oxidation of ozone-PVDF hybrid membrane |
| CN105316973A (en) * | 2015-12-08 | 2016-02-10 | 中国科学院青岛生物能源与过程研究所 | Preparation process of pulping prehydrolysis liquid based on advanced oxidation-nanofiltration technology |
| CN105350369A (en) * | 2015-12-08 | 2016-02-24 | 中国科学院青岛生物能源与过程研究所 | Preparation process of lignocellulose pulping pre-hydrolysis liquid having efficient fermentation capability |
| CN105420312A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing food-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105624337A (en) * | 2016-01-07 | 2016-06-01 | 江苏振宇环保科技有限公司 | Method for preparing xylose functional sugar by hemicellulose polysaccharide in hydrolyzed agricultural wastes |
| CN105648120A (en) * | 2015-12-31 | 2016-06-08 | 常州市长宇实用气体有限公司 | Method for preparing xylose functional sugar from hemicellulose polysaccharide in hydrolyzed agricultural waste |
| CN205527942U (en) * | 2016-01-25 | 2016-08-31 | 英诺伟霆（北京）环保技术有限公司 | Inner loop ozone catalytic unit |
| CN206127003U (en) * | 2016-05-06 | 2017-04-26 | 上海宝钢化工有限公司 | Improved generation ozone catalytic oxidation device |
| CN106893788A (en) * | 2017-04-14 | 2017-06-27 | 四川金象赛瑞化工股份有限公司 | A kind of method that hemicellulose is prepared xylose by continuous stream micro passage reaction |
| CN106977616A (en) * | 2017-03-28 | 2017-07-25 | 暨南大学 | A kind of method that utilization hydrogen peroxide oxidation edman degradation Edman prepares flaxseed gum oligosaccharide |
-
2017
- 2017-08-31 CN CN201710773954.XA patent/CN107475466B/en active Active
Patent Citations (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62281890A (en) * | 1986-05-29 | 1987-12-07 | Norin Suisansyo Ringyo Shikenjo | Production of xylose and xylooligosaccharide |
| CN201136844Y (en) * | 2007-12-07 | 2008-10-22 | 山东福田药业有限公司 | Neutralization device for hydrolysate in production of xylose |
| CN101649570A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Process for preparing wheatgrass cellulose with low pollution |
| CN101787398A (en) * | 2010-01-22 | 2010-07-28 | 中国科学院过程工程研究所 | Method for purifying, reclaiming and condensing sugar in lignocellulose prehydrolysis liquid |
| CN101962213A (en) * | 2010-10-21 | 2011-02-02 | 东南大学 | Energy-saving multitube photochemical excitation/oxidation water advanced treatment device |
| CN102643935A (en) * | 2012-04-11 | 2012-08-22 | 宜宾丝丽雅股份有限公司 | Method for preparing xylose by using squeezed waste alkali liquor in viscose fiber production process |
| CN102899426A (en) * | 2012-10-25 | 2013-01-30 | 浙江华康药业股份有限公司 | Method for preparing xylose by using dissolving pulp wood chip prehydrolysis liquid |
| CN103074790A (en) * | 2012-12-25 | 2013-05-01 | 济南圣泉集团股份有限公司 | Comprehensive utilization process of biomass raw material |
| CN103898246A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Method for producing xylose by using biomass raw material |
| CN103898247A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Technology for producing xylose from biomass raw materials |
| CN103193896A (en) * | 2013-03-12 | 2013-07-10 | 武汉纤浓生物科技有限公司 | Method of preparing konjac glucomannan and thin film evaporator used therein |
| CN104109722A (en) * | 2014-07-01 | 2014-10-22 | 丽水学院 | Preparation method for xylo-oligosaccharide |
| CN104404108A (en) * | 2014-12-09 | 2015-03-11 | 齐鲁工业大学 | Pre-treating method for improving sugar conversion rate of lignocellulose |
| CN204752442U (en) * | 2015-06-26 | 2015-11-11 | 青岛科技大学 | Catalysis ozone oxidation promoters |
| CN105060458A (en) * | 2015-07-21 | 2015-11-18 | 黑龙江大学 | Water-purification device by utilizing catalytic oxidation of ozone-PVDF hybrid membrane |
| CN105316973A (en) * | 2015-12-08 | 2016-02-10 | 中国科学院青岛生物能源与过程研究所 | Preparation process of pulping prehydrolysis liquid based on advanced oxidation-nanofiltration technology |
| CN105350369A (en) * | 2015-12-08 | 2016-02-24 | 中国科学院青岛生物能源与过程研究所 | Preparation process of lignocellulose pulping pre-hydrolysis liquid having efficient fermentation capability |
| CN105420312A (en) * | 2015-12-15 | 2016-03-23 | 宜宾雅泰生物科技有限公司 | Method for preparing food-grade xylo-oligosaccharide through viscose squeezed alkali liquid |
| CN105648120A (en) * | 2015-12-31 | 2016-06-08 | 常州市长宇实用气体有限公司 | Method for preparing xylose functional sugar from hemicellulose polysaccharide in hydrolyzed agricultural waste |
| CN105624337A (en) * | 2016-01-07 | 2016-06-01 | 江苏振宇环保科技有限公司 | Method for preparing xylose functional sugar by hemicellulose polysaccharide in hydrolyzed agricultural wastes |
| CN205527942U (en) * | 2016-01-25 | 2016-08-31 | 英诺伟霆（北京）环保技术有限公司 | Inner loop ozone catalytic unit |
| CN206127003U (en) * | 2016-05-06 | 2017-04-26 | 上海宝钢化工有限公司 | Improved generation ozone catalytic oxidation device |
| CN106977616A (en) * | 2017-03-28 | 2017-07-25 | 暨南大学 | A kind of method that utilization hydrogen peroxide oxidation edman degradation Edman prepares flaxseed gum oligosaccharide |
| CN106893788A (en) * | 2017-04-14 | 2017-06-27 | 四川金象赛瑞化工股份有限公司 | A kind of method that hemicellulose is prepared xylose by continuous stream micro passage reaction |
Non-Patent Citations (3)
| Title |
|---|
| 丁长河等: "微波处理对玉米芯酶法制备低聚木糖的影响", 《河南工业大学学报(自然科学版)》 * |
| 叶利培等: "木聚糖酶水解竹材废弃物制取低聚木糖工艺条件的优化", 《食品工业科技》 * |
| 魏承厚等: "木糖制备技术研究进展", 《广西轻工业》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107475466B (en) | 2020-12-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104818640B (en) | Bioanalysis extracts Plant fiber's manufacturing technique method | |
| CN105623861B (en) | A kind of glycerine esterification reaction unit | |
| CN106087513A (en) | A kind of fractionation method of sulfate-reducing conditions | |
| CN203750367U (en) | Waste gas treating and recycling device | |
| CN114702056A (en) | Method for absorbing carbon dioxide in power plant tail gas by desulfurized gypsum | |
| CN109499253A (en) | A kind of damaged tire refining equipment waste gas dedusting system | |
| CN205088084U (en) | Mud separation processing device | |
| CN107475466A (en) | The technique that a kind of ozone acid hydrolyzed hemicellulose prepares xylose | |
| CN206828868U (en) | A kind of combination unit for separating cellulose, lignin and carbohydrate | |
| CN207259420U (en) | The equipment that a kind of ozone acid hydrolyzed hemicellulose prepares xylose | |
| CN211005382U (en) | System for anaerobic fermentation produces marsh gas and retrieves sulphur | |
| CN109505179A (en) | Stalk low-carbon technology for hydrolyzing | |
| KR101282830B1 (en) | Production Method of Solubility Pulp Made From Dioscorea batatas | |
| CN206278931U (en) | A kind of acetylene cleaning Waste Sulfuric Acid processing equipment | |
| CN109504724A (en) | Stalk cleans co-production technology | |
| CN105420309B (en) | A kind of pretreating process improving grass family raw cellulose enzymatic saccharification rate | |
| CN209519535U (en) | A kind of damaged tire refining equipment waste gas dedusting system | |
| CN207958409U (en) | Pressure sending type cyclonic separation acidolysis cellulose pretreatment unit | |
| CN204261648U (en) | A kind of filtering type sulfur melting kettle | |
| KR101282831B1 (en) | Solubility Pulp Made From Dioscorea batatas | |
| CN107245505B (en) | Multistage hydrolysis saccharification method for urban waste biomass resources | |
| CN206288970U (en) | A kind of thio conversion ammonium sulfate process equipment of desulphurization waste liquid of coke oven gas salt extraction | |
| CN207520766U (en) | A kind of boiler exhaust gas processing utilizes device | |
| CN205419831U (en) | Result separation and drying equipment of nitromethane building -up reactions | |
| CN214882577U (en) | Preprocessing device of crops discarded object wax layer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |