CN109651527A - The method of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide - Google Patents
The method of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide Download PDFInfo
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- CN109651527A CN109651527A CN201811277880.1A CN201811277880A CN109651527A CN 109651527 A CN109651527 A CN 109651527A CN 201811277880 A CN201811277880 A CN 201811277880A CN 109651527 A CN109651527 A CN 109651527A
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- algal polysaccharides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
Abstract
The present invention provides a kind of methods of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide, comprising the following steps: S1, the titanium dioxide optical catalyst for providing marine algae powder and doping ferro element are spare；Seawood meal is dissolved in the water by S2, and passes through Ultrasonic Wave-Assisted Extraction and be centrifuged, and collects upper layer algal polysaccharides supernatant；The upper layer algal polysaccharides supernatant is carried out dissolved oxygen processing, obtains algal polysaccharides pretreatment fluid by S3；S4, will be added the titanium dioxide optical catalyst of catalytic amount in the algal polysaccharides pretreatment fluid, sufficiently illumination and auxiliary ultrasonic degradation in whipping process obtains algal polysaccharides degradation solution；The algal polysaccharides degradation solution is centrifugally separating to obtain degradation supernatant, and filtered by S5, is finally freeze-dried and functional oligosaccharide is made.
Description
Technical field
The present invention relates to a kind of methods of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide.
Background technique
Currently, the artificial breeding of seaweed is very universal in the world, and yield is big.In China, seaweed industry has obtained considerable
Development, seaweed total output occupies the nearly half in the world, while also increasingly various by the processed side product type that it is derived.In recent years
, the comprehensive exploitation of polysaccharide is more and more studied and is paid close attention to utilization in seaweed.Wherein, it is prepared by algal polysaccharides
Oligosaccharides have multiple biological activities, such as low energy, reducing blood lipid, it is anti-oxidant, antitumor, adjust flora, agricultural, health care food
Product, medicine and other fields have broad application prospects.In addition, seaweed is cheap and easy to get, the algal polysaccharides degree of polymerization is relatively low, easy drop
Solution, makes seaweed show great potential in terms of the preparation of oligosaccharides.
Containing polysaccharide such as algin, fucoidin, seaweed starch in algal polysaccharides, and based on algin, fucoidin
Want ingredient.Algin is a kind of anionic acid polysaccharide, is passed through by α-L- guluronic acid (G) and beta-D-mannuronic acid (M)
The linear polysaccharide of 1-4 glucosides bond disorder connection, is primarily present in the brown algas such as sargassum, bulk kelp, some bacteriums can also secrete
Algin.Algin oligosaccharide is the oligomer of algin, and relative molecular weight is low, has good water solubility, stability height, safe nothing
The physicochemical property of poison.Fucoidin is a kind of using fucose as the composite sulfur of main constituents acidification polysaccharide.It is a kind of spy
Different polysaccharide, the molecule chain end at it contain sulfate group.Just because of the presence of natural sulphur acidic group, fucoidin could table
Reveal excellent, apparent physiological activity.Research has shown that fucoidin is not a kind of compound of single structure, but has not
With a compounds of group of chemical constituent.Fucoidin oligosaccharides has bioactive functions more abundant, such as removes free radical, resists
Thrombus, antiviral, anticoagulation, blood pressure lowering etc..
Tradition degradation algal polysaccharides method is mainly chemical degradation method and enzymatic isolation method.In addition, physical method is as a kind of simple
Quick preparation method is concerned by people.It is worth noting that, the oligosaccharide structure of distinct methods preparation is different.For
For algin, what is obtained by enzymatic isolation method is unsaturated oligosaccharide, and what chemical degradation method obtained is that saturation uronic acid is few
Sugar, while its relative molecular mass and G/M ratio also determine its physicochemical property and bioactivity.Chemical degradation method is with acid drop
Based on solution, production cost is low, technology maturation, but production process needs irritation chemical reagent, and there are corrosive equipments, reagent
Recycle the problems such as difficulty pollutes environment and oligosaccharides yield is lower, and molecular weight is difficult to control.Enzymatic isolation method reacts mild, green high-efficient,
But production cost is higher.Physical method is simple and quick by high temperature and pressure degradation algal polysaccharides based on hydro-thermal method, but produces
Journey energy consumption is big, the high requirements on the equipment.
The light of polysaccharide especially algal polysaccharides urges degradation report relatively fewer, and principle and all light urge degradation of organic substances
Process is similar, is the glycosidic bond that the attacks such as hydroxyl radical free radical, ultra-oxygen anion free radical fracture algal polysaccharides are generated by photocatalysis,
To obtain low molecular weight oligosaccharides.Ultrasonic wave supplementary means generates certain destroy to seaweed tissue, cell due to its cavitation
Effect, can further dissolve out intracellular polysaccharide, while accelerate to dissolve iuntercellular polysaccharide.
Currently, having the scientific documents of a small amount of photoactivation and ultrasonic wave added degradation algal polysaccharides both at home and abroad, technique is only
Algal polysaccharides can be degraded to higher molecular weight, i.e. 20000 dalton or so.
Summary of the invention
The present invention provides a kind of methods of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide, can effectively solve
The certainly above problem.
The present invention is implemented as follows:
A kind of method of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide, comprising the following steps:
S1, the titanium dioxide optical catalyst for providing marine algae powder and doping ferro element are spare；
Seawood meal is dissolved in the water by S2, and passes through Ultrasonic Wave-Assisted Extraction and be centrifuged, and collects upper layer algal polysaccharides supernatant
Liquid；
The upper layer algal polysaccharides supernatant is carried out dissolved oxygen processing, obtains algal polysaccharides pretreatment fluid by S3；
The titanium dioxide optical catalyst of catalytic amount will be added in S4 in the algal polysaccharides pretreatment fluid, stirred
Abundant illumination and auxiliary ultrasonic degradation, obtain algal polysaccharides degradation solution in journey；
The algal polysaccharides degradation solution is centrifugally separating to obtain degradation supernatant, and filtered by S5, and finally freeze-drying is made
Functional oligosaccharide.
As further improved, in step sl, the marine algae powder passes through following steps and obtains:
S11, by new fresh seaweed or processing fent cleaning removal silt and impurity, and by after ether defatting 50~60
DEG C drying to constant weight, is finally sieved.
As further improved, in step sl, the titanium dioxide optical catalyst passes through following steps and obtains:
Mica is mixed in water according to solid-to-liquid ratio 1:5~15, and hydrochloric acid titanium tetrachloride solution is added dropwise by S12, reaction temperature
Degree is 50~80 DEG C, and controlling pH value by dilute alkaline soln is 1.8~2.5, is sufficiently reacted；And
S13 instills acid ferric sulfate or ferric chloride solution in reaction system, 80~90 DEG C of temperature, and molten by diluted alkaline
Hydraulic control pH value is 3~3.5, and the titanium dioxide optical catalyst for adulterating ferro element is prepared in sufficiently reaction.
As further improved, in step s 12, the partial size of the mica is 10~30 microns.
It is in step s 2, described that seawood meal is dissolved in the water as further improved, and pass through ultrasonic wave assisted Leaching
It mentions and includes: the step of centrifugation
Seawood meal deionized water is dissolved in the water with weight ratio for 1:50~80 by S21, and passes through ultrasonic wave assisted Leaching
It mentions 10~30 minutes, ultrasonic power is 100~1000W, and Extracting temperature is 30~60 DEG C.
It is in step s3, described that the upper layer algal polysaccharides supernatant is subjected to dissolved oxygen processing as further improved
The step of include:
Rotor is added in the upper layer algal polysaccharides supernatant by S31, uses flow pumps logical with the rate of 10~15ml/min
Enter air, and is promoted dissolved oxygen 5~30 minutes with rotor with the revolving speed of 50~600r/min.
As further improved, in step s 4, the optically catalytic TiO 2 that weight ratio is 0.1~1% is added
Agent.
As further improved, in step s 4, the reaction temperature of the abundant illumination and auxiliary ultrasonic degradation are as follows:
Xenon lamp power is 100~1000W, ultrasonic power is 200~1000W, and temperature is 30~60 DEG C, and degradation time is 0.5~24
Hour.
As further improved, the method further includes step S6:
It will be added after the undegraded constituents mixt recycling of the catalyst residue and seaweed that are obtained by filtration in the step S5
New catalytic degradation process.
The beneficial effects of the present invention are: photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide provided by the invention
The method algal polysaccharides that can quickly and effectively degrade to obtain functional oligosaccharide can effectively inhibit E. coli Activity,
Part oligosaccharides also has anti-tumor activity.It is 3~50 additionally by the functional oligosaccharide degree of polymerization made from this method, phase
It is 600~10000 dalton to molecular weight distribution.In addition, to mix ferro element modified for the titanium dioxide in the present invention, in addition to close purple
Outskirt is still active, can also bring the activity response of visible region 400~600nm range, make this technology there is a possibility that with day
Right sunlight carries out catalytic degradation, keeps production process more environmentally protective.Finally, the present invention is rationally degraded using a variety of physical methods
Algal polysaccharides, reaction process does not add chemical reagent, and final catalyst physical filtering can return easily due to being insoluble solids
Receive, it is more more economical than conventional method environmental protection, rapidly and efficiently, it is relatively low to equipment requirement.
Detailed description of the invention
It, below will be to use required in embodiment in order to illustrate more clearly of the technical solution of embodiment of the present invention
Attached drawing be briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not to be seen as
It is the restriction to range, it for those of ordinary skill in the art, without creative efforts, can be with root
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the method flow of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide provided in an embodiment of the present invention
Figure.
Specific embodiment
To keep the purposes, technical schemes and advantages of embodiment of the present invention clearer, implement below in conjunction with the present invention
The technical solution in embodiment of the present invention is clearly and completely described in attached drawing in mode, it is clear that described reality
The mode of applying is some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention, ability
Domain those of ordinary skill every other embodiment obtained without creative efforts, belongs to the present invention
The range of protection.Therefore, the detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit below and is wanted
The scope of the present invention of protection is sought, but is merely representative of selected embodiment of the invention.Based on the embodiment in the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this
Invent the range of protection.
Shown in referring to Fig.1, a kind of method of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide, including following step
It is rapid:
S1, the titanium dioxide optical catalyst for providing marine algae powder and doping ferro element are spare；
Seawood meal is dissolved in the water by S2, and passes through Ultrasonic Wave-Assisted Extraction and be centrifuged, and collects upper layer algal polysaccharides supernatant
Liquid；
The upper layer algal polysaccharides supernatant is carried out dissolved oxygen processing, obtains algal polysaccharides pretreatment fluid by S3；
The titanium dioxide optical catalyst of catalytic amount will be added in S4 in the algal polysaccharides pretreatment fluid, stirred
Abundant illumination and auxiliary ultrasonic degradation, obtain algal polysaccharides degradation solution in journey；
The algal polysaccharides degradation solution is centrifugally separating to obtain degradation supernatant, and filtered by S5, and finally freeze-drying is made
Functional oligosaccharide.
In step sl, the marine algae powder is obtained by following steps:
S11, by new fresh seaweed or processing fent cleaning removal silt and impurity, and by after ether defatting 50~60
DEG C drying to constant weight, is finally sieved.
The titanium dioxide optical catalyst can be obtained by following steps:
Mica is mixed in water according to solid-to-liquid ratio 1:5~15, and hydrochloric acid titanium tetrachloride solution is added dropwise by S12, reaction temperature
Degree is 50~80 DEG C, and controlling pH value by dilute alkaline soln is 1.8~2.5, is sufficiently reacted；And
S13 instills acid ferric sulfate or ferric chloride solution in reaction system, 80~90 DEG C of temperature, and molten by diluted alkaline
Hydraulic control pH value is 3~3.5, and the titanium dioxide optical catalyst for adulterating ferro element is prepared in sufficiently reaction.
In step s 12, the partial size of the mica is preferably 10~30 microns.The concentration of the hydrochloric acid titanium tetrachloride solution
For 1.0mol/L~3.0mol/L.The dilute alkaline soln is dilute sodium hydroxide.And the reaction time are as follows: 1~12 hour.In step
In S13, the concentration of the acidity ferric sulfate or ferric chloride solution is 0.1mol/L~1.0mol/L.And the reaction time are as follows: 1~9
Hour.In step s 2, described that seawood meal is dissolved in the water, and pass through Ultrasonic Wave-Assisted Extraction and include: the step of centrifugation
Seawood meal deionized water is dissolved in the water with weight ratio for 1:50~80 by S21, and passes through ultrasonic wave assisted Leaching
It mentions 10~30 minutes, ultrasonic power is 100~1000W, and Extracting temperature is 30~60 DEG C.
In step s3, the described the step of upper layer algal polysaccharides supernatant is carried out dissolved oxygen processing, includes:
Rotor is added in the upper layer algal polysaccharides supernatant by S31, uses flow pumps logical with the rate of 10~15ml/min
Enter air, and is promoted dissolved oxygen 5~30 minutes with rotor with the revolving speed of 50~600r/min.In step s 4, weight ratio is added is
0.1~1% titanium dioxide optical catalyst.The reaction temperature of the abundant illumination and auxiliary ultrasonic degradation are as follows: xenon
Lamp power is 100~1000W, ultrasonic power is 200~1000W, and temperature is 30~60 DEG C, and degradation time is 0.5~24 hour.
As further improved, the method can further include step S6:
It will be added after the undegraded constituents mixt recycling of the catalyst residue and seaweed that are obtained by filtration in the step S5
New catalytic degradation process.
Embodiment 1
(1) prepared by raw material: new fresh seaweed or its processing fent cleaning removal silt, impurity, 60 DEG C of bakings after ether defatting
It does to constant weight, smashes it through 120 meshes, it is spare to obtain seawood meal；
(2) preparation of titanium dioxide optical catalyst: adulterate ferro element titanium dioxide optical catalyst be by partial size be 10~
30 μm of mica sheet is substrate, and the solid-to-liquid ratio of mica and water is 1:10, by 2.0mol/L hydrochloric acid titanium tetrachloride solution with 1.5ml/
Min flow velocity instills reaction system, 75 DEG C of temperature, controls PH=2.0 with diluted sodium hydroxide solution, reacts 6h, then by 0.5mol/L
Acid ferrum sulfuricum oxydatum solutum instills reaction system with 1.0ml/min flow velocity, 85 DEG C of temperature, controls PH=with diluted sodium hydroxide solution
3.2~3.3,5h is reacted, is prepared that quality is uniform, pearlescent pigment of golden color；
(3) extract algal polysaccharides: by the seawood meal obtained by step (1) with deionized water with weight ratio be 1:70 stirring fill
Point dissolution be placed on ultrasonic wave added extraction 30min, ultrasonic power 500w, Extracting temperature be 45 DEG C, then by lysate with
4000r/min is centrifuged 10min, collects algal polysaccharides supernatant；
(4) centrifuged supernatant pre-processes: rotor is added in the polysaccharide supernatant obtained by step (3), using flow pumps
It is passed through air with the rate of 15ml/min, and dissolved oxygen 10min is promoted with the revolving speed of 300r/min with rotor, it is pre- to obtain algal polysaccharides
Treatment fluid；
(5) photocatalysis ultrasonic wave added degradation algal polysaccharides: weight ratio, which is added, in the pretreatment fluid obtained by step (4) is
5 ‰ titanium dioxide optical catalysts obtained by step (2), and with rotor be dispersed with stirring uniformly, xenon source power be 350w,
Ultrasonic power is 350w, temperature is that the 2h that degrades at 45 DEG C (takes every reaction 30min taking-up reaction solution, with rotor by titanium dioxide
Photochemical catalyst is dispersed with stirring uniformly), obtain algal polysaccharides degradation solution；
(6) purifying degradation solution prepares oligosaccharides: will be centrifuged by the degradation solution that step (5) obtain with the revolving speed of 6000r/min
20min obtains degradation supernatant, after 0.45 μm of filter membrane to remove photochemical catalyst titanium dioxide, finally freezes filtrate dry
Dry obtained functional oligosaccharide product.
Embodiment 2
(1) prepared by raw material: new fresh seaweed or its processing fent cleaning removal silt, impurity, 60 DEG C of bakings after ether defatting
It does to constant weight, smashes it through 80 meshes, it is spare to obtain seawood meal；
(2) preparation of titanium dioxide optical catalyst: adulterate ferro element titanium dioxide optical catalyst be by partial size be 10~
30 μm of mica sheet is substrate, and the solid-to-liquid ratio of mica and water is 1:10, by 2.0mol/L hydrochloric acid titanium tetrachloride solution with 1.5ml/
Min flow velocity instills reaction system, 75 DEG C of temperature, controls PH=2.0 with diluted sodium hydroxide solution, reacts 6h, then by 0.5mol/L
Acid ferrum sulfuricum oxydatum solutum instills reaction system with 1.0ml/min flow velocity, 85 DEG C of temperature, controls PH=with diluted sodium hydroxide solution
3.2~3.3,5h is reacted, is prepared that quality is uniform, pearlescent pigment of golden color；
(3) extract algal polysaccharides: by the seawood meal obtained by step (1) with deionized water with weight ratio be 1:80 stirring fill
Point dissolution be placed on ultrasonic wave added extraction 30min, ultrasonic power 800w, Extracting temperature be 60 DEG C, then by lysate with
4000r/min is centrifuged 10min, collects algal polysaccharides supernatant；
(4) centrifuged supernatant pre-processes: rotor is added in the polysaccharide supernatant obtained by step (3), using flow pumps
It is passed through air with the rate of 15ml/min, and dissolved oxygen 10min is promoted with the revolving speed of 300r/min with rotor, it is pre- to obtain algal polysaccharides
Treatment fluid；
(5) photocatalysis ultrasonic wave added degradation algal polysaccharides: weight ratio, which is added, in the pretreatment fluid obtained by step (4) is
8 ‰ titanium dioxide optical catalysts obtained by step (2), and with rotor be dispersed with stirring uniformly, xenon source power be 350w,
Ultrasonic power is 350w, temperature is that the 3h that degrades at 60 DEG C (takes every reaction 30min taking-up reaction solution, with rotor by titanium dioxide
Photochemical catalyst is dispersed with stirring uniformly), obtain algal polysaccharides degradation solution；
(6) purifying degradation solution prepares oligosaccharides: will be centrifuged by the degradation solution that step (5) obtain with the revolving speed of 6000r/min
20min obtains degradation supernatant, after 0.45 μm of filter membrane to remove photochemical catalyst titanium dioxide, finally freezes filtrate dry
Dry obtained functional oligosaccharide product.
Embodiment 3
(1) prepared by raw material: new fresh seaweed or its processing fent cleaning removal silt, impurity, 60 DEG C of bakings after ether defatting
It does to constant weight, smashes it through 160 meshes, it is spare to obtain seawood meal；
(2) preparation of titanium dioxide optical catalyst: adulterate ferro element titanium dioxide optical catalyst be by partial size be 10~
30 μm of mica sheet is substrate, and the solid-to-liquid ratio of mica and water is 1:10, by 2.0mol/L hydrochloric acid titanium tetrachloride solution with 1.5ml/
Min flow velocity instills reaction system, 75 DEG C of temperature, controls PH=2.0 with diluted sodium hydroxide solution, reacts 6h, then by 0.5mol/L
Acid ferrum sulfuricum oxydatum solutum instills reaction system with 1.0ml/min flow velocity, 85 DEG C of temperature, controls PH=with diluted sodium hydroxide solution
3.2~3.3,5h is reacted, is prepared that quality is uniform, pearlescent pigment of golden color；
(3) extract algal polysaccharides: by the seawood meal obtained by step (1) with deionized water with weight ratio be 1:60 stirring fill
Point dissolution be placed on ultrasonic wave added extraction 30min, ultrasonic power 1000w, Extracting temperature be 30 DEG C, then by lysate with
4000r/min is centrifuged 10min, collects algal polysaccharides supernatant；
(4) centrifuged supernatant pre-processes: rotor is added in the polysaccharide supernatant obtained by step (3), using flow pumps
It is passed through air with the rate of 15ml/min, and dissolved oxygen 10min is promoted with the revolving speed of 300r/min with rotor, it is pre- to obtain algal polysaccharides
Treatment fluid；
(5) photocatalysis ultrasonic wave added degradation algal polysaccharides: weight ratio, which is added, in the pretreatment fluid obtained by step (4) is
2 ‰ titanium dioxide optical catalysts obtained by step (2), and with rotor be dispersed with stirring uniformly, xenon source power be 350w,
Ultrasonic power is 350w, temperature is that the 2.5h that degrades at 30 DEG C (takes every reaction 30min taking-up reaction solution, with rotor by titanium dioxide
Titanium photochemical catalyst is dispersed with stirring uniformly), obtain algal polysaccharides degradation solution；
(6) purifying degradation solution prepares oligosaccharides: will be centrifuged by the degradation solution that step (5) obtain with the revolving speed of 6000r/min
20min obtains degradation supernatant, after 0.45 μm of filter membrane to remove photochemical catalyst titanium dioxide, finally freezes filtrate dry
Dry obtained functional oligosaccharide product.
The functional oligosaccharide degree of polymerization being prepared by the method for the invention is 3~50, relative molecular weight distribution 600
~10000.In addition, the functional oligosaccharide that the present invention is prepared can effectively inhibit E. coli Activity, part oligosaccharides has
Anti-tumor activity and good moisturizing, moisture absorption activity.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of method of photocatalysis ultrasonic wave added degradation seaweed preparation functional oligosaccharide, which comprises the following steps:
S1, the titanium dioxide optical catalyst for providing marine algae powder and doping ferro element are spare；
Seawood meal is dissolved in the water by S2, and passes through Ultrasonic Wave-Assisted Extraction and be centrifuged, and collects upper layer algal polysaccharides supernatant；
The upper layer algal polysaccharides supernatant is carried out dissolved oxygen processing, obtains algal polysaccharides pretreatment fluid by S3；
The titanium dioxide optical catalyst of catalytic amount will be added, in whipping process in S4 in the algal polysaccharides pretreatment fluid
Abundant illumination and auxiliary ultrasonic degradation, obtain algal polysaccharides degradation solution；
The algal polysaccharides degradation solution is centrifugally separating to obtain degradation supernatant, and filtered by S5, is finally freeze-dried and function is made
Property oligosaccharides.
2. the method as described in claim 1, which is characterized in that in step sl, the marine algae powder is obtained by following steps
:
S11, by new fresh seaweed or processing fent cleaning removal silt and impurity, and by being dried after ether defatting at 50~60 DEG C
It does to constant weight, is finally sieved.
3. the method as described in claim 1, which is characterized in that in step sl, the titanium dioxide optical catalyst by with
Lower step obtains:
Mica is mixed in water according to solid-to-liquid ratio 1:5~15, and hydrochloric acid titanium tetrachloride solution is added dropwise by S12, and reaction temperature is
50~80 DEG C, and controlling pH value by dilute alkaline soln is 1.8~2.5, is sufficiently reacted；And
S13 instills acid ferric sulfate or ferric chloride solution in reaction system, 80~90 DEG C of temperature, and passes through dilute alkaline soln control
PH value processed is 3~3.5, and the titanium dioxide optical catalyst for adulterating ferro element is prepared in sufficiently reaction.
4. the method as described in claim 1, which is characterized in that in step s 12, the partial size of the mica is 10~30 micro-
Rice.
5. the method as described in claim 1, which is characterized in that it is in step s 2, described that seawood meal is dissolved in the water, and lead to
It crosses Ultrasonic Wave-Assisted Extraction and includes: the step of centrifugation
Seawood meal deionized water is dissolved in the water with weight ratio for 1:50~80 by S21, and passes through Ultrasonic Wave-Assisted Extraction 10
~30 minutes, ultrasonic power was 100~1000W, and Extracting temperature is 30~60 DEG C.
6. the method as described in claim 1, which is characterized in that in step s3, described by the upper layer algal polysaccharides supernatant
Liquid carry out dissolved oxygen processing the step of include:
The upper layer algal polysaccharides supernatant is added rotor, flow pumps is used to be passed through sky with the rate of 10~15ml/min by S31
Gas, and promoted dissolved oxygen 5~30 minutes with rotor with the revolving speed of 50~600r/min.
7. the method as described in claim 1, which is characterized in that in step s 4, be added weight ratio be 0.1~1% it is described
Titanium dioxide optical catalyst.
8. the method as described in claim 1, which is characterized in that in step s 4, the abundant illumination and auxiliary ultrasonic drop
The reaction temperature of solution are as follows: xenon lamp power is 100~1000W, ultrasonic power is 200~1000W, and temperature is 30~60 DEG C, drop
Solving the time is 0.5~24 hour.
9. the method as described in claim 1, which is characterized in that further comprise step S6:
It will be added newly after the undegraded constituents mixt recycling of the catalyst residue and seaweed that are obtained by filtration in the step S5
Catalytic degradation process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004431A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Method for photocatalytic degradation of fucoidin and application of product thereof in antibiosis |
| CN114318374A (en) * | 2022-01-06 | 2022-04-12 | 大连工业大学 | Method for degrading hyaluronic acid based on titanium dioxide modified ITO electrode photoelectrocatalysis |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899686A (en) * | 2006-07-24 | 2007-01-24 | 同济大学 | Process for preparing iron blended TiO2/active carbon composite visible light catalyst |
| CN101219371A (en) * | 2007-01-08 | 2008-07-16 | 北京化工大学 | Photocatalysis oxidation treated high concentration organic trade waste |
| CN103265645A (en) * | 2013-06-03 | 2013-08-28 | 浙江宇翔生物科技有限公司 | Device and method for extracting algal polysaccharide by ultrasonic-assisted extraction |
| CN107325589A (en) * | 2017-07-05 | 2017-11-07 | 江苏贝丽得新材料有限公司 | A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof |
-
2018
- 2018-10-30 CN CN201811277880.1A patent/CN109651527A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1899686A (en) * | 2006-07-24 | 2007-01-24 | 同济大学 | Process for preparing iron blended TiO2/active carbon composite visible light catalyst |
| CN101219371A (en) * | 2007-01-08 | 2008-07-16 | 北京化工大学 | Photocatalysis oxidation treated high concentration organic trade waste |
| CN103265645A (en) * | 2013-06-03 | 2013-08-28 | 浙江宇翔生物科技有限公司 | Device and method for extracting algal polysaccharide by ultrasonic-assisted extraction |
| CN107325589A (en) * | 2017-07-05 | 2017-11-07 | 江苏贝丽得新材料有限公司 | A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof |
Non-Patent Citations (8)
| Title |
|---|
| JANKANA BURANA-OSOT 等: "photolytic depolymerization of alginate", 《CARBOHYDRATE RESEARCH》 * |
| MOHAMMAD TAGHI TAGHIZADEH 等: "Sonolytic, sonocatalytic and sonophotocatalytic degradation of chitosan", 《ULTRASONICS SONOCHEMISTRY》 * |
| 包景岭等: "《恶臭环境管理与污染控制》", 31 December 2009, 中国环境科学出版社 * |
| 徐蕾 等: "《负载型多酸光催化材料及应用》", 31 March 2015, 东北师范大学出版社 * |
| 杜尧国等: "《光催化剂纳米二氧化钛的改性研究》", 30 September 2007, 吉林大学出版社 * |
| 段振华: "《高级食品化学》", 31 January 2012, 中国轻工业出版社 * |
| 沈玉龙 等: "《绿色化学》", 31 August 2014, 华中科技大学出版社 * |
| 白春华: "《非金属矿物基二氧化钛制备、改性及废水处理技术》", 31 December 2015, 中国矿业大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113004431A (en) * | 2021-03-03 | 2021-06-22 | 大连工业大学 | Method for photocatalytic degradation of fucoidin and application of product thereof in antibiosis |
| CN114318374A (en) * | 2022-01-06 | 2022-04-12 | 大连工业大学 | Method for degrading hyaluronic acid based on titanium dioxide modified ITO electrode photoelectrocatalysis |
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