CN104861115B - A kind of preparation method of anionic glucan flocculant - Google Patents
A kind of preparation method of anionic glucan flocculant Download PDFInfo
- Publication number
- CN104861115B CN104861115B CN201510070055.4A CN201510070055A CN104861115B CN 104861115 B CN104861115 B CN 104861115B CN 201510070055 A CN201510070055 A CN 201510070055A CN 104861115 B CN104861115 B CN 104861115B
- Authority
- CN
- China
- Prior art keywords
- glucan
- solution
- flocculant
- anionic
- ethanol
- 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.)
- Active
Links
Abstract
The invention provides a kind of preparation method of anionic glucan flocculant, methods described includes：Step 1, the ethyl sodium buffer preparation sucrose solution using pH5.0, dextransucrase is added in the sucrose solution and carries out enzymic catalytic reaction, until the dynamic viscosity of reaction solution reaches 8000~10000CPS, terminate enzymic catalytic reaction, it is soluble in water after being settled out macromolecule glucan and washing, obtain the macromolecule dextran solution that solid content is 5~10%；Under step 2, oxygen free condition, potassium peroxydisulfate is added into macromolecule dextran solution and is used as initiator with sodium hydrogensulfite, it is incubated at 50 DEG C~70 DEG C after 15~20min, sodium acrylate solution is added as anionic monomer and carries out graft copolymerization, terminate the graft copolymerization, go out to be grafted crude product using ethanol precipitation, it is multiple soluble in water after being washed through ethanol, that is, the anionic glucan flocculant of milky thick liquid nano is made.
Description
Technical field
The present invention relates to biological flocculant field, more particularly to a kind of preparation side of anionic glucan flocculant
Method.
Background technology
With industry develop rapidly and population growth, increasing surface and ground water is by different degrees of
Pollution, water quality deterioration, shortage of water resources have been today's society huge difficult problems in the urgent need to address.In water treatment field, wadding
Solidifying technology is the step process using most also most criticals, and the height of flocculation efficiency depends primarily on the choosing of flocculant species
Select.In the past few decades, some organic polymer (such as polyacrylamides of inorganic flocculating agent (aluminium salt and molysite etc.) with synthesis
Amine) it is widely used in flocculation operation, but also result in serious secondary pollution and new environmental problem.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of non-harmful anionic glucan flocculation of environmental protection
The preparation method of agent.
It is described the invention discloses a kind of preparation method of anionic glucan flocculant in order to solve the above problems
Method includes：
Step 1, acetic acid-sodium acetate buffer solution preparation sucrose solution using pH5.0, are added in the sucrose solution
Dextransucrase, at 26~28 DEG C, carries out enzymic catalytic reaction 24~28 hours, until the dynamic viscosity of reaction solution reaches
8000~10000CPS, terminates the enzymic catalytic reaction, soluble in water after being settled out macromolecule glucan and washing, admittedly contained
Measure the macromolecule dextran solution for 5~10%；
Under step 2, oxygen free condition, it is (1 that molar concentration ratio is added into the macromolecule dextran solution：10)~
(4:1) potassium peroxydisulfate, as initiator, is incubated after 15~20min with sodium hydrogensulfite at 50 DEG C~70 DEG C, adds propylene
Acid sodium solution carries out graft copolymerization 2~4 hours as anionic monomer, the graft copolymerization is terminated, using ethanol
Grafting crude product is settled out, multiple soluble in water after being washed through ethanol, that is, the anionic Portugal that milky thick liquid nano is made gathers
Sugared flocculant.
Preferably, described dextransucrase is obtained by leuconostoc mesenteroide and spine spore mould mixed fungus fermentation.
When preferably, using dextransucrase catalysing sucrose solution, the molar concentration of the sucrose for 0.2~
1.0mol/L, the concentration of the dextransucrase are 0.5~3.0U/mL.
Preferably, the molar concentration of the potassium peroxydisulfate is 0.1~1.0mmol/L, the sodium hydrogensulfite it is mole dense
Spend for 0.25~1.0mmol/L.
Preferably, methods described also includes：
Freeze-dried powder is made in the anionic glucan flocculant of the milky thick liquid nano；
Or, 45~55 DEG C of baking ovens are placed in after 45% ethanol cyclic washing to prepared anionic glucan flocculant
In be dried overnight, obtain white dried solid particle.
Preferably, in the graft copolymerization, the molar concentration of the PAA is 0.05~0.20mol/L, institute
The volume ratio for stating boiomacromolecule glucan and the PAA is 1：1.
Preferably, acetic acid-sodium acetate buffer solution of the pH5.0 is used to be configured to molar concentration for 0.2~1.0mol/
The L sucrose solution；
The termination enzymic catalytic reaction includes：
Enzymic catalytic reaction is terminated by the way of heating and thermal insulation；
It is described be settled out macromolecule glucan and wash after step soluble in water include：
Go out macromolecule glucan with 95% ethanol precipitation after cooling, sediment is washed with 45% ethanol, finally will
It is dissolved in distilled water.
Preferably, the termination graft copolymerization includes：
The graft copolymerization is terminated by cooling down；
The use ethanol precipitation goes out to be grafted crude product, after being washed through ethanol it is multiple it is soluble in water including：
Go out to be grafted crude product using 95% ethanol precipitation, after 45% ethanol cyclic washing, redissolve in distilled water.
Compared with prior art, the present invention includes advantages below：
By the embodiment of the present invention, first using dextransucrase catalysing sucrose solution, it is made highly viscous biological high
Molecule dextran solution；Then under anaerobic, the redox initiation system constituted in potassium peroxydisulfate and sodium hydrogensulfite
It is interior, using gained boiomacromolecule glucan as substrate, using PAA as anionic monomer, graft copolymerization is carried out, is obtained
The anionic derivative of glucan, as anionic glucan flocculant.
Glucan is innovatively applied to field of Environment Protection by the embodiment of the present invention, and the graft copolymerization of boiomacromolecule is applied to
The derivatization of glucan, obtained glucan graft product can be as a kind of excellent boiomacromolecule flocculant, for locating
Manage all kinds of water pollution problems.
Compared with commercially available organic flocculant, the flocculant safety non-toxic of the embodiment of the present invention is nuisanceless, without any to environment
There is the composition of harm, realize industrialized production and the application of green bio flocculant.Also, based on the basic of boiomacromolecule
Skeleton structure, the derivative after grafting still can regenerate, it is possible to biodegradable, meet the Ecological View of sustainable development.Cause
This, this high compatibility causes glucan derivative flocculant to have in terms of heavy metal environmental pollution with reference to the hypotoxicity of itself
Very big application prospect.
In addition, the solution process step of the embodiment of the present invention is simple, the preparation technology cycle is short, and low in raw material price.
Through concrete application, the anionic glucan flocculant flocculation activity prepared using the scheme of the embodiment of the present invention
Height, consumption is few, is especially up to 99% to the turbidity removal rate of aqueous suspension ofkaolin, and can be used cooperatively with other flocculants, place
Manage all kinds of water pollution problems.
Brief description of the drawings
Fig. 1 is a kind of preparation method flow chart of anionic glucan flocculant of the present invention；
Fig. 2 be the embodiment of the present invention example 1 in anionic glucan flocculant infrared spectrogram；
Fig. 3 be the embodiment of the present invention example 1 in anionic glucan flocculant freeze-dried powder X-ray crystal diffraction
Figure.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, with reference to embodiment
The present invention is further detailed explanation.
Experimental method described in following embodiments, is conventional method unless otherwise specified；The reagent and material,
Unless otherwise specified, commercially obtain.
The problem of there is pollution environment in inorganic flocculating agent and organic flocculant, and belong to can be again for natural polymerses
Production-goods source, possesses these advantageous advantages such as easy to use, easy degraded, non-secondary pollution, however, most of natural height
Molecular substance surface charge is weak, molecular weight is not high enough, poorly water-soluble, it is therefore desirable to which boiomacromolecule is chemically modified, this
Invention proposes a kind of preparation method of anionic glucan flocculant.
Reference picture 1, it illustrates a kind of preparation method of anionic glucan flocculant described in the embodiment of the present invention
Flow chart, methods described can specifically include：
Step 101, acetic acid-sodium acetate buffer solution preparation sucrose solution using pH5.0, add in the sucrose solution
Plus dextransucrase, at 26~28 DEG C, enzymic catalytic reaction is carried out 24~28 hours, until the dynamic viscosity of reaction solution reaches
8000~10000CPS, terminates the enzymic catalytic reaction, soluble in water after being settled out macromolecule glucan and washing, admittedly contained
Measure the macromolecule dextran solution for 5~10%.
In the scheme of the embodiment of the present invention, first using dextransucrase catalysing sucrose solution, obtained dynamic viscosity is
8000~10000CPS boiomacromolecule dextran solution.Enzyme-catalyzed reaction condition is gentle, energy consumption is low, using acetic acid-acetic acid
Sodium strictly controls the pH of reaction solution to be 5.0, and in order to ensure the purity of macromolecule glucan, it is necessary to control the reaction time so that
The dynamic viscosity of reaction solution is in 8000~10000CPS.
Under step 102, oxygen free condition, it is (1 that molar concentration ratio is added into the macromolecule dextran solution：10)~
(4:1) potassium peroxydisulfate, as initiator, is incubated after 15~20min with sodium hydrogensulfite at 50 DEG C~70 DEG C, adds propylene
Acid sodium solution carries out graft copolymerization 2~4 hours as anionic monomer, the graft copolymerization is terminated, using ethanol
Grafting crude product is settled out, multiple soluble in water after being washed through ethanol, that is, the anionic Portugal that milky thick liquid nano is made gathers
Sugared flocculant.
The embodiment of the present invention is after obtained boiomacromolecule dextran solution, further, in potassium peroxydisulfate and bisulfite
Sodium constitute redox initiation system in, using above-mentioned gained boiomacromolecule glucan as substrate, using PAA for the moon from
Sub- monomer, carries out graft copolymerization, obtains the anionic derivative of glucan, as anionic glucan flocculant.
Glucan is the polysaccharide of first industrialized production in the world, by glucose unit by α -1,6- glycosidic bonds and α -
1,3- glycosidic bond is formed by connecting, and is the boiomacromolecule that a class has important commercial value, be widely used in medicine, food and
Chemical field.Glucan is applied to field of Environment Protection by present invention innovation, and the graft copolymerization of boiomacromolecule is applied into glucan
Derivatization, obtained glucan graft product to metal ion (such as silver, mercury, copper) have high affinity, can conduct
A kind of excellent boiomacromolecule flocculant, for handling all kinds of water pollution problems, also, this high compatibility combines itself
Hypotoxicity cause glucan derivative to have very big application prospect in terms of heavy metal environmental pollution.
In flocculation operation, flocculant mainly realizes the improvement of water quality by two kinds of mechanism：One kind is charge neutrality effect,
That is the opposite charges of ionic group (quaternary ammonium salt, carboxylate radical etc.) institute band of flocculating agent molecule can significantly shield miscellaneous in the aqueous solution
The electric double layer of matter particulate matter, so as to destroy the aggregation between impurity particle thing；Another is adsorption bridging effect, i.e. HMW
Biological flocculant with water-soluble form in the presence of, with big hydration particle diameter, different suspended particulate substances can be built bridge
Form connect.However, most of natural high molecular substance surface charges are weak, molecular weight is not high enough, poorly water-soluble, therefore
Need to be chemically modified boiomacromolecule.
Innovation of the embodiment of the present invention proposes to be chemically modified macromolecule dextran solution using graft copolymerization, with
Boiomacromolecule flocculating properties are improved, the characteristic group in grafted monomers is introduced by boiomacromolecule by graft copolymerization
In, increase the conformational freedom of boiomacromolecule, so as to improve its adsorption bridging and charge neutrality ability.Based on boiomacromolecule
Basic skeleton structure, the derivative after grafting still can regenerate, it is possible to biodegradable, meet the ecology of sustainable development
See.Therefore, this high compatibility causes glucan derivative flocculant in heavy metal environmental pollution with reference to the hypotoxicity of itself
Aspect has very big application prospect.
In addition, the solution process step of the embodiment of the present invention is simple, the preparation technology cycle is short, and low in raw material price.
Through concrete application, the anionic glucan flocculant flocculation activity prepared using the scheme of the embodiment of the present invention
Height, consumption is few, is especially up to 99% to the turbidity removal rate of aqueous suspension ofkaolin, and can be used cooperatively with other flocculants, place
Manage all kinds of water pollution problems.
In the embodiment of the present invention, it is preferable that described dextransucrase is by leuconostoc mesenteroide and spine spore mould
Obtained by mixed fungus fermentation, mixed fungus fermentation raw material is simple, easy to operate, can produce the dextransucrase of high enzyme activity, high stability.
In the embodiment of the present invention, it is preferable that during using dextransucrase catalysing sucrose solution, according to dextransucrase
Height continue catalytic mechanism, the molar concentration of the sucrose be preferably 0.2~1.0mol/L, the dextransucrase it is dense
Degree is preferably 0.5~3.0U/mL.
In the embodiment of the present invention, it is preferable that the molar concentration of the potassium peroxydisulfate can be 0.1~1.0mmol/L, described
The molar concentration of sodium hydrogensulfite can be 0.25~1.0mmol/.
Described anionic glucan flocculant can have three kinds of existence forms：Milky thick liquid, white dried
Particle, white lyophilized powder.In the embodiment of the present invention, it is preferable that methods described can also include：By the milky viscous fluid
Freeze-dried powder is made in the anionic glucan flocculant of body shape；Or, to prepared anionic glucan flocculant through 45%
It is placed in 45~55 DEG C of baking ovens and is dried overnight after ethanol cyclic washing, obtains white dried solid particle.
In the embodiment of the present invention, it is preferable that in the graft copolymerization, the molar concentration of the PAA is 0.05
The volume ratio of~0.20mol/L, the boiomacromolecule glucan and the PAA is 1：1, to prevent implode phenomenon, really
Protect the high efficiency of graft copolymerization.
In the embodiment of the present invention, it is preferable that be configured to using acetic acid-sodium acetate buffer solution of the pH5.0 mole dense
Spend the sucrose solution for 0.2~1.0mol/L.
In the embodiment of the present invention, it is preferable that the termination enzymic catalytic reaction can include：Using the side of heating and thermal insulation
Formula terminates enzymic catalytic reaction, it is ensured that the complete deactivation of enzyme molecule.
In the embodiment of the present invention, it is preferable that the termination graft copolymerization can include：Lead to overcooled mode
Free radical polymerization rate can be reduced rapidly, and then terminates the graft copolymerization.
In the embodiment of the present invention, it is preferable that it is described be settled out macromolecule glucan and wash after step soluble in water can
With including：Go out macromolecule glucan with 95% ethanol precipitation after cooling, sediment is washed with 45% ethanol, washed as far as possible
Remove low-molecular polysaccharide, it is ensured that the purity of macromolecule glucan, be finally dissolved in distilled water.
In the embodiment of the present invention, it is preferable that the use ethanol precipitation goes out to be grafted crude product, redissolved after being washed through ethanol in
It can include in water：Go out to be grafted crude product using 95% ethanol precipitation, through 45% ethanol cyclic washing, it is ensured that low molecular homopolymerization
Thing and other small-molecule substances are kept completely separate with product, finally redissolve precipitation in distilled water.
To make those skilled in the art more fully understand the present invention, specifically illustrate the present invention's below by way of multiple
A kind of preparation method of anionic glucan flocculant.
Example 1
First, 0.2mol/L sucrose solution is prepared using pH5.0 acetic acid-sodium acetate buffer solution, by sucrose solution
Catalytic reaction is carried out under the conditions of 26 DEG C of stirring in water bath 24 hours with 1.5U/mL dextransucrase, obtain 8000CPS height
Molecule glucan；Obtained glucan (about 100mL) is then loaded to the necks of 250mL tri- that mechanical stirring device is closed with condenser pipe
In reaction bulb (solid content is about 10%), it is abundant that 60 DEG C of stirrings are allowed to dissolving；Again by 0.1mmol/L potassium peroxydisulfate with
1.0mmol/L sodium hydrogensulfite (being used as redox initiation system) is slowly added in three-necked bottle, is incubated 15min；Then
100mL 0.1mol/L PAAs are added in three neck reaction bulbs, 50 DEG C are stirred polymerisation 4 hours, and last alcohol precipitation is simultaneously collected
Precipitation i.e. obtain milky graft product, while will precipitation rinsed repeatedly with 45% ethanol and distilled water respectively afterwards redissolve in
In distilled water, the anionic glucan flocculant of milky thick liquid nano is obtained.
Graft product obtained above is subjected to kaolin active testing：Kaolin is made into 0.5% with running water first
Suspension 200mL, stand 10min after ultrasonic dissolution assisting 10min, take a certain amount of supernatant (actually turbid solution) to measure OD550=
1.458, it is designated as A0；Then above-mentioned graft product is diluted to the solution that solid content is about 0.5%, and added under agitating device
400 μ L solid contents be 0.5% anionic glucan flocculant, stirring 5min after stand 10min and observe settling of floccus show
As then drawing a certain amount of supernatant and measuring OD550=0.028, it is designated as A；Finally calculate flocculating rate F=(A0- A) ÷ A0
× 100%=98.1%.
The infrared spectrogram of anionic glucan flocculant in the example 1 of the embodiment of the present invention is shown with reference to Fig. 2, it is right
Than glucan and its derivative collection of illustrative plates can be seen that graft reaction after, the infrared absorption peak of the combination water of glucan in itself
1649cm-1Disappear, the substitute is the absworption peak 1721cm of carboxylic acid C=O structures-1, illustrate anionic monomer acrylic acid sodium with
Glucan is successfully made graft copolymerization；
Show that the X-ray of anionic glucan flocculant freeze-dried powder in the example 1 of the embodiment of the present invention is brilliant with reference to Fig. 3
The crystallogram of body diffraction pattern, contrast glucan and graft product is it can be found that substrate glucan has 2 θ=15 °, 17 °,
Five kinds of absworption peaks at 18 °, 20 ° and 2 θ=29 °, show typical A- types X-ray diffraction pattern, and is connect with PAA
The XRD spectrum of branch product only shows scattered broad peak, it is meant that the reduction of crystallinity, while illustrating drawing for sodium acrylate monomers
Enter to change the ordered structure inside dextran molecule, further demonstrate that glucan is successfully carried out with anionic monomer acrylic acid sodium
Graft copolymerization.
Example 2
First, 0.5mol/L sucrose solution is prepared using pH5.0 acetic acid-sodium acetate buffer solution, by sucrose solution
Catalytic reaction is carried out under the conditions of 26 DEG C of stirring in water bath 28 hours with 0.5U/mL dextransucrase, obtain 9000CPS height
Molecule glucan；Obtained glucan (about 100mL) is then loaded to the necks of 250mL tri- that mechanical stirring device is closed with condenser pipe
In reaction bulb (solid content is about 5%), it is abundant that 60 DEG C of stirrings are allowed to dissolving；Again by 1.0mmol/L potassium peroxydisulfate with
0.25mmol/L sodium hydrogensulfite (being used as redox initiation system) is slowly added in three-necked bottle, is incubated 18min；Then will
100mL 0.2mol/L PAAs are added in three neck reaction bulbs, and 65 DEG C are stirred polymerisation 3 hours, and it is heavy that last alcohol precipitation is simultaneously collected
Form sediment and obtain milky graft product, while being redissolved after precipitation is rinsed repeatedly with 45% ethanol and distilled water respectively in steaming
In distilled water, the anionic glucan flocculant of milky thick liquid nano is obtained.
Graft product obtained above is subjected to kaolin active testing：Kaolin is made into 0.5% with running water first
Suspension 200mL, stand 10min after ultrasonic dissolution assisting 10min, take a certain amount of supernatant (actually turbid solution) to measure OD550=
1.508, it is designated as A0；Then above-mentioned graft product is diluted to the solution that solid content is about 0.5%, and to height under agitating device
10min is stood after the anionic glucan flocculant that 400 μ L solid contents of addition are 0.5% in the soil suspension of ridge, stirring 5min
And settling of floccus phenomenon is observed, then draw a certain amount of supernatant and measure OD550=0.018, it is designated as A；Finally calculate flocculation
Rate F=(A0- A) ÷ A0× 100%=98.8%.
Example 3
First, 1.0mol/L sucrose solution is prepared using pH5.0 acetic acid-sodium acetate buffer solution, by sucrose solution
Catalytic reaction is carried out under the conditions of 28 DEG C of stirring in water bath 24 hours with 3.0U/mL dextransucrase, obtain 8500CPS height
Molecule glucan；Obtained glucan (about 100mL) is then loaded to the necks of 250mL tri- that mechanical stirring device is closed with condenser pipe
In reaction bulb (solid content is about 8%), it is abundant that 60 DEG C of stirrings are allowed to dissolving；Again by 0.8mmol/L potassium peroxydisulfate with
0.4mmol/L sodium hydrogensulfite (being used as redox initiation system) is slowly added in three-necked bottle, is incubated 20min；Then
100mL 0.05mol/L PAAs are added in three neck reaction bulbs, 70 DEG C are stirred polymerisation 2 hours, and last alcohol precipitation is simultaneously received
Collection precipitation obtains milky graft product, while being redissolved after precipitation is rinsed repeatedly with 45% ethanol and distilled water respectively
In distilled water, the anionic glucan flocculant of milky thick liquid nano is obtained.
Graft product obtained above is subjected to kaolin active testing：Kaolin is made into 1% with running water first
10min is stood after suspension 200mL, ultrasonic dissolution assisting 10min, takes a certain amount of supernatant (actually turbid solution) to measure OD550=
1.658, it is designated as A0；Then above-mentioned graft product is diluted to the solution that solid content is about 0.5%, and to height under agitating device
10min is stood after the addition anionic glucan flocculants of 400 μ L 0.5% in the soil suspension of ridge, stirring 5min and observes flco
Sedimentation phenomenon, then draws a certain amount of supernatant and measures OD550=0.066, it is designated as A；Finally calculate flocculating rate F=(A0-
A)÷A0× 100%=96%.
Example 4
First, 0.5mol/L sucrose solution is prepared using pH5.0 acetic acid-sodium acetate buffer solution, by sucrose solution
Catalytic reaction is carried out under the conditions of 27 DEG C of stirring in water bath 26 hours with 1.0U/mL dextransucrase, obtain 10000CPS's
Macromolecule glucan；Obtained glucan (about 100mL) is then loaded to the 250mL tri- that mechanical stirring device is closed with condenser pipe
In neck reaction bulb (solid content is about 6%), it is abundant that 60 DEG C of stirrings are allowed to dissolving；Again by 0.5mmol/L potassium peroxydisulfate with
0.5mmol/L sodium hydrogensulfite (being used as redox initiation system) is slowly added in three-necked bottle, is incubated 20min；Then
100mL 0.1mol/L PAAs are added in three neck reaction bulbs, 60 DEG C are stirred polymerisation 4 hours, and last alcohol precipitation is simultaneously collected
Precipitation i.e. obtain milky graft product, while will precipitation rinsed repeatedly with 45% ethanol and distilled water respectively afterwards redissolve in
In distilled water, the anionic glucan flocculant of milky thick liquid nano is obtained.
Graft product obtained above is subjected to kaolin active testing：Kaolin is made into 1% with running water first
10min is stood after suspension 200mL, ultrasonic dissolution assisting 10min, takes a certain amount of supernatant (actually turbid solution) to measure OD550=
1.625, it is designated as A0；Then above-mentioned graft product is diluted to the solution that solid content is about 0.5%, and to height under agitating device
10min is stood after the addition anionic glucan flocculants of 400 μ L 0.5% in the soil suspension of ridge, stirring 5min and observes flco
Sedimentation phenomenon, then draws a certain amount of supernatant and measures OD550=0.016, it is designated as A；Finally calculate flocculating rate F=(A0-
A)÷A0× 100%=99%.
The preferred embodiment cited by the present invention is these are only, and is not used to limit the scope of the invention, affiliated skill
Equivalent modification or change that those of ordinary skill in art field is made with the present invention, it is same to belong to the patent of the present invention
Protection domain.
For embodiment of the method, in order to be briefly described, therefore it is all expressed as to a series of combination of actions, but this area
Technical staff should know that the present invention is not limited by described sequence of movement, because according to the present invention, some steps can
To carry out using other orders or simultaneously.Secondly, those skilled in the art should also know, described in this description to implement
Example belongs to preferred embodiment, and involved action and the part not necessarily present invention are necessary.
A kind of preparation method of anionic glucan flocculant provided by the present invention is described in detail above,
Specific case used herein is set forth to the principle and embodiment of the present invention, and the explanation of above example is to use
Understand the method and its core concept of the present invention in help；Simultaneously for those of ordinary skill in the art, according to the present invention's
Thought, will change in specific embodiments and applications, in summary, and this specification content should not be construed as
Limitation of the present invention.
Claims (6)
1. a kind of preparation method of anionic glucan flocculant, it is characterised in that methods described includes：
Step 1, acetic acid-sodium acetate buffer solution preparation sucrose solution using pH5.0, add Portugal poly- in the sucrose solution
Sucrase enzyme, at 26~28 DEG C, carries out enzymic catalytic reaction 24~28 hours, until the dynamic viscosity of reaction solution reach 8000~
10000CPS, terminates the enzymic catalytic reaction, soluble in water after being settled out macromolecule glucan and washing, and it is 5 to obtain solid content
~10% macromolecule dextran solution, described dextransucrase is to mix bacterium hair by leuconostoc mesenteroide and spine spore mould
Obtained by ferment, the molar concentration of sucrose is that 0.2~1.0mol/L, the concentration of the dextransucrase are in the sucrose solution
0.5~3.0U/mL；
Under step 2, oxygen free condition, it is 1 that molar concentration ratio is added into the macromolecule dextran solution：10~4:1 mistake
Potassium sulfate, as initiator, is incubated after 15~20min with sodium hydrogensulfite at 50 DEG C~70 DEG C, and addition sodium acrylate solution is made
Graft copolymerization is carried out for anionic monomer 2~4 hours, terminates the graft copolymerization, grafting is gone out using ethanol precipitation
Crude product, it is multiple soluble in water after being washed through ethanol, that is, the anionic glucan flocculant of milky thick liquid nano is made.
2. according to the method described in claim 1, it is characterised in that the molar concentration of the potassium peroxydisulfate is 0.1~
1.0mmol/L, the molar concentration of the sodium hydrogensulfite is 0.25~1.0mmol/L.
3. according to the method described in claim 1, it is characterised in that methods described also includes：
Freeze-dried powder is made in the anionic glucan flocculant of the milky thick liquid nano；
Or, prepared anionic glucan flocculant is placed in after 45% ethanol cyclic washing in 45~55 DEG C of baking ovens dry
It is dry to stay overnight, obtain white dried solid particle.
4. according to the method described in claim 1, it is characterised in that in the graft copolymerization, the sodium acrylate solution
Molar concentration be 0.05~0.20mol/L, the volume of the boiomacromolecule dextran solution and the sodium acrylate solution
Than for 1：1.
5. according to the method described in claim 1, it is characterised in that：
Acetic acid-sodium acetate buffer solution of the pH5.0 is used to be configured to the sucrose of the molar concentration for 0.2~1.0mol/L
Solution；
The termination enzymic catalytic reaction includes：
Enzymic catalytic reaction is terminated by the way of heating and thermal insulation；
It is described be settled out macromolecule glucan and wash after step soluble in water include：
Go out macromolecule glucan with 95% ethanol precipitation after cooling, sediment is washed with 45% ethanol, it is finally that its is molten
In distilled water.
6. according to the method described in claim 1, it is characterised in that：
The termination graft copolymerization includes：
The graft copolymerization is terminated by cooling down；
The use ethanol precipitation goes out to be grafted crude product, after being washed through ethanol it is multiple it is soluble in water including：
Go out to be grafted crude product using 95% ethanol precipitation, after 45% ethanol cyclic washing, redissolve in distilled water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510070055.4A CN104861115B (en) | 2015-02-10 | 2015-02-10 | A kind of preparation method of anionic glucan flocculant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510070055.4A CN104861115B (en) | 2015-02-10 | 2015-02-10 | A kind of preparation method of anionic glucan flocculant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104861115A CN104861115A (en) | 2015-08-26 |
| CN104861115B true CN104861115B (en) | 2017-09-15 |
Family
ID=53907338
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510070055.4A Active CN104861115B (en) | 2015-02-10 | 2015-02-10 | A kind of preparation method of anionic glucan flocculant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104861115B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105132390B (en) * | 2015-09-28 | 2018-05-01 | 合肥工业大学 | A kind of method that dextransucrase is prepared using mixed fungus fermentation |
| CN110437378A (en) * | 2019-09-09 | 2019-11-12 | 安徽春霖环保科技有限公司 | Cationic dextran based polyalcohol, preparation and the application as flocculant |
| JP2023528442A (en) * | 2020-06-04 | 2023-07-04 | ニュートリション・アンド・バイオサイエンシーズ・ユーエスエー・フォー，インコーポレイテッド | Dextran-α-glucan graft copolymer and its derivative |
| CN112920404B (en) * | 2021-01-29 | 2023-01-24 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN114874445B (en) * | 2022-04-29 | 2023-09-19 | 合肥工业大学智能制造技术研究院 | Preparation method and application of dextran-polyaspartic acid anionic flocculant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392280A (en) * | 2007-09-18 | 2009-03-25 | 庄茅 | Enzymology method for preparing polysaccharide bioflocculant |
| CN103834574A (en) * | 2014-01-03 | 2014-06-04 | 合肥工业大学 | Dextranase and application of same in preparation of low molecular dextran |
| CN104327215A (en) * | 2014-11-14 | 2015-02-04 | 威海汉邦生物环保科技有限公司 | Ultra-high molecular weight anion biological polysaccharide grafted copolymer and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1693391A4 (en) * | 2003-12-03 | 2007-07-18 | Toagosei Co Ltd | Process for producing water-soluble polymer |
| EP2138560B2 (en) * | 2008-06-24 | 2015-04-01 | Cognis IP Management GmbH | Cleaner containing graft copolymers |
-
2015
- 2015-02-10 CN CN201510070055.4A patent/CN104861115B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101392280A (en) * | 2007-09-18 | 2009-03-25 | 庄茅 | Enzymology method for preparing polysaccharide bioflocculant |
| CN103834574A (en) * | 2014-01-03 | 2014-06-04 | 合肥工业大学 | Dextranase and application of same in preparation of low molecular dextran |
| CN104327215A (en) * | 2014-11-14 | 2015-02-04 | 威海汉邦生物环保科技有限公司 | Ultra-high molecular weight anion biological polysaccharide grafted copolymer and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104861115A (en) | 2015-08-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104861115B (en) | A kind of preparation method of anionic glucan flocculant | |
| CN109553701B (en) | Preparation method of modified chitosan polymer | |
| Mittal et al. | Flocculation characteristics and biodegradation studies of Gum ghatti based hydrogels | |
| CN103724455A (en) | Hyaluronic acid derivative and preparation method for hyaluronic acid hydrogel | |
| CN107141387A (en) | A kind of method that controllable free-radical pickering emulsion polymerization prepares polymer | |
| CN102344526B (en) | Preparation method of branched polystyrene-maleic anhydride and application thereof | |
| CN104045778B (en) | Preparation method of star-like hybrid material with UCST and polyhedral oligomeric silsesquioxane (POSS) as core | |
| CN104292475A (en) | Temperature-sensitive and photosensitive dual-response polypeptide based host-guest composite intelligent hydrogel as well as preparation method and application thereof | |
| Anjum et al. | Microwave irradiated copolymerization of xanthan gum with acrylamide for colonic drug delivery | |
| CN106009003A (en) | Injectable self-repairing hydrogel based on polysaccharides, preparation method and application of hydrogel to biological tissue engineering | |
| Sahu et al. | Microwave mediated rapid synthesis of chitosan | |
| CN107915848A (en) | A kind of preparation method of chitin whisker/hydroxyl butyl chitosan temperature-sensitive hydrogel | |
| CN103709309A (en) | Preparation method of salt-resistant water-absorbent resin with high water absorption rate | |
| CN110437378A (en) | Cationic dextran based polyalcohol, preparation and the application as flocculant | |
| CN102051332A (en) | Collection method of oil-containing microalgae | |
| CN109021168A (en) | A method of caused using plasma and synthesizes chitosan-based flocculant | |
| Wang et al. | Synthesis and characterization of a cationic dextran-based flocculant and its application in bacterial sedimentation | |
| Yang et al. | Preparation, flocculation and application in sugar refining of eco-friendly dextran-polylysine complex flocculant | |
| CN105585695A (en) | Method for preparing poly-caprolactone-lactide in supercritical carbon dioxide in random copolymerization mode | |
| Klein et al. | Preparation of cashew gum-based flocculants by microwave-and ultrasound-assisted methods | |
| CN104987513A (en) | Preparing method for sugar responsive magnetic hybridization nano particles | |
| CN103214587A (en) | Method for processing composite modified starch by employing ultrasonic technology | |
| CN102229923B (en) | Lipase nano-sized polymer biocatalyst particle and preparation method thereof | |
| CN102250278A (en) | pH-sensitive renewable polymer for water-soluble immobilized cellulase as well as preparation method and application thereof | |
| CN101361976B (en) | Hyaluronic acid modified polu-cyano acrylic acid alkyl ester nano granules and preparation method and use thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |