CN110437378A - Cationic dextran based polyalcohol, preparation and the application as flocculant - Google Patents
Cationic dextran based polyalcohol, preparation and the application as flocculant Download PDFInfo
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- CN110437378A CN110437378A CN201910845854.2A CN201910845854A CN110437378A CN 110437378 A CN110437378 A CN 110437378A CN 201910845854 A CN201910845854 A CN 201910845854A CN 110437378 A CN110437378 A CN 110437378A
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- flocculant
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation methods of cationic dextran based polyalcohol, it is under anaerobic, potassium peroxydisulfate is added into dextran solution and stirs 15-20min, addition METAC reacts 2-4h at 65-75 DEG C, ethyl alcohol is added to be precipitated, it is dry after purifying washing, obtain white dried solid particle, as cationic dextran based polyalcohol, the dextran solution are to obtain sucrose solution by the enzymatic fermentation reaction of dextransucrase.Compared with commercially available organic flocculant, flocculant of the invention is safe and non-toxic nuisanceless, without the harmful ingredient of any pair of environment, realizes the industrialized production and application of green bio flocculant.Also, the basic skeleton structure based on boiomacromolecule, the derivative after grafting still can regenerate, and have good biodegradable and biocompatibility, meet the Ecological View of sustainable development.
Description
Technical field
The present invention relates to biological polyoses base flocculant fields, more particularly to a kind of cationic dextran derivative class
Flocculant and preparation method thereof.
Background technique
With the rapid development of industry and the growth of population, more and more surface and ground waters are 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 to apply a step process of most also most criticals, and the height of flocculation efficiency depends primarily on the choosing of flocculant type
It selects.In the past few decades, some organic polymer (such as polyacrylamides of inorganic flocculating agent (aluminium salt and molysite etc.) and synthesis
Amine) it is widely used in flocculation operation, but also result in serious secondary pollution and new environmental problem.And source
From biomass material, the natural polysaccharide of marine resources and microorganism as synthetic polymer product have good reactivity and
Environment friendly is quickly becoming the feasibility substitute for the organic high molecular polymer being harmful to the human body.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of environmentally protective, biodegradable cationic dextroses
Anhydride group polymer, preparation and the application as flocculant in water pollutant processing.
A kind of preparation method of cationic dextran based polyalcohol of the invention, is under anaerobic, to the right
It revolves and potassium peroxydisulfate stirring 15-20min is added in sugared anhydride solution, addition METAC reacts 2-4h at 65-75 DEG C, and ethyl alcohol is added and obtains
It must precipitate, it is dry after purifying washing, obtain white dried solid particle, as cationic dextran based polyalcohol.
In the preparation method of cationic dextran based polyalcohol described above, it is preferred that the dextran solution
It is to obtain sucrose solution by the enzymatic fermentation reaction of dextransucrase.It can specifically be prepared via a method which: adopt
With acetic acid-calcium acetate buffer preparation sucrose solution of pH=5.0-5.5, dextran sugarcane is added in the sucrose solution
Carbohydrase carries out enzymatic fermentation reaction, and reaction to dynamic viscosity reaches 8000-10000CPS at 20-28 DEG C, terminates reaction, adopts
It is with ethyl alcohol alcohol precipitation high molecular weight dextran and soluble in water after washing 2-3 times, it is right to obtain the macromolecule that solid content is 5-10%
Revolve sugared anhydride solution.Wherein, the dextransucrase is a kind of hydrolysis that dextran is catalyzed and synthesized using sucrose as substrate
Synzyme can be generated to be well known in the art by leuconostoc mesenteroide, or being capable of high expression dextran sucrase
The genetic engineering bacterium of enzyme generates such as Chinese patent CN101363009A, or sharp as described in Chinese patent CN105132390A
It is prepared and is generated with mixed fungus fermentation.
The molar concentration of the sucrose solution is 0.55~0.75mol/L, is acetic acid-second using pH=5.0-5.5
Sour calcium buffer preparation obtains, and the concentration of the dextransucrase is 5.0~6.0U/mL.
In the preparation method of cationic dextran based polyalcohol described above, it is preferred that the potassium peroxydisulfate adds
Enter amount for the 3% of dextran quality as radical initiator.
In the preparation method of cationic dextran based polyalcohol described above, it is preferred that the METAC and dextrose
The molar ratio of acid anhydride is 3:1.
The cationic dextrose anhydride group that the preparation method of cationic dextran based polyalcohol described above obtains is poly-
Closing object can be used as flocculant application.
Preferably, it can be applied in water pollutant processing as flocculant, the water pollutant can be inorganic
Impurity such as kaolin etc., or the anionic component or the macromolecular components with anionic group etc..
Preferably, the application as flocculant in sugar industry.
Preferably, the application as flocculant in dyestuff contaminant processing.
Preferably, because it is cationic flocculant, therefore it is used especially for anions component or with yin
The flocculation treatment of the macromolecular components of ionic group.
Preparation method of the present invention is catalyzed sucrose reaction solution by dextransucrase first, ferments and high viscosity is made
Dextran biological polyoses liquid；Then under anaerobic, using potassium peroxydisulfate as radical initiator, with gained biology
High molecular dextran is substrate, with 2- (methacryloxy)-ethyl-trimethyl salmiac (METAC) for cation mono
Body carries out graft copolymerization, obtains cationic dextran radical derivative, as a kind of cationic dextran flocculation
Agent.
Dextran is innovatively applied to environment protection field by the present invention, and the graft copolymerization of boiomacromolecule is applied to dextrorotation
The derivative reaction of sugared acid anhydride, obtained dextran cationization graft product, it is high to can be used as a kind of biology of good performance
Molecular flocculant, for handling in water body containing water pollutants such as anion, band anionic group macromoleculars.
Compared with commercially available organic flocculant, flocculant of the invention is safe and non-toxic nuisanceless, harmful without any pair of environment
Ingredient, realize the industrialized production and application of green bio flocculant.Also, the basic framework knot based on boiomacromolecule
Structure, the derivative after grafting have good biodegradable and biocompatibility, meet the Ecological View of sustainable development.Cause
This, this dextran derivative class flocculant anion waste water, dye discoloration and in terms of have it is very big
Application prospect.
In addition, the operating procedure step of the scheme of the embodiment of the present invention is simple, the preparation process period is short, product quality is controllable
And low in raw material price.Although polysaccharide itself be it is biodegradable and usually than synthesis organic flocculant it is more stable,
But they usually show lower flocculation activity and need higher flocculant dose.The present invention is copolymerized using chemical graft
Method carries out modification to polysaccharide and improves flocculation efficiency, flocculating property.
Through concrete application, the cationic dextran flocculant flocculability prepared using the scheme of the embodiment of the present invention
Can be high, dosage is few, and pH scope of application width is 5-9.It, can be high to the turbidity removal rate of aqueous suspension ofkaolin when water pH value is 7
It up to 97.8%, and can be used cooperatively with other flocculants, handle waste water pollution problem.Attached drawing 1 is pH value in reaction to graft product
The influence of flocculating property.As we can clearly see from the figure under the conditions of neutral environment, i.e., when pH value in reaction is 7, dextrorotation at this time
Sugared acid anhydride cationization graft product is best to the flocculation efficiency of Kaolin clay suspension, can reach 97.8% and remove turbidity.And dextrorotation
Degradation has occurred in acid condition for sugared acid anhydride itself will lead to grafting rate less than to influence the final flocculating property of product.And
In alkaline environment, the carbon atom that quaternary ammonium salt group entrained by grafted monomers METAC is connected is vulnerable to attack so as to cause it
It is unstable and be easily decomposed to not carry the group of cationic charge, so as to cause the reduction of final product flocculation activity.
Detailed description of the invention
Fig. 1 is influence of the pH value in reaction to graft product flocculating property；
Fig. 2 is a kind of reaction mechanism figure of cationic dextran flocculant of the invention；
Fig. 3 is the infrared spectrogram of cationic dextran flocculant in the example 1 of the embodiment of the present invention；
Fig. 4 is the X-ray crystallogram of cationic dextran flocculant in the example 1 of the embodiment of the present invention.
Fig. 5 is flocculating effect display diagram: aqueous suspension ofkaolin flocculating effect, and a left side is preceding suspension-muddiness of flocculating, has largely
Suspended particulate substance, to add, flocculating effect-solution after flocculant of the present invention is clarified, suspended particulate substance is flocculated sedimentation on the right side.
Fig. 6 flocculant dose of the present invention influences the flocculation of sugar-cane juice.
Specific embodiment
Embodiment 1
Firstly, using acetic acid-calcium acetate buffer preparation 0.58mol/L sucrose solution of pH=5.4, sucrose is anti-
It answers solution to carry out catalystic, fermentative under the conditions of T=25 DEG C of stirring in water bath with the dextransucrase of 5.0U/mL to react 24 hours,
Reaction to dynamic viscosity reaches 8000CPS, using ethyl alcohol alcohol precipitation high molecular weight dextran and soluble in water after washing 2-3 times,
Obtain the high molecular dextran solution that solid content is 5-10%；Then obtained dextran solution (about 100mL) is packed into
It is abundant to be allowed to dissolution for stirring in tri- neck reaction flask of 250mL with mechanical stirring device；Again by the potassium peroxydisulfate of 3% mass content
(causing system as radical initiator) is slowly added in three-necked bottle, in T=60 DEG C of initiation 15min；Then cation mono is pressed
Body 2- (methacryloxy)-ethyl-trimethyl salmiac (METAC) is 3:1 (mol/ with the molar ratio of reacting of dextran
Mol METAC monomer) is added, is stirred polymerization reaction 3 hours at T=60 DEG C, is eventually adding 95% ethyl alcohol and collects precipitating, if
Precipitating with 50% ethyl alcohol repeated flushing and then is redissolved in distilled water, the sun of milky thick liquid nano can be obtained
Ionic dextrose anhydride group flocculant；If 50% ethyl alcohol repeated flushing will be precipitated and then is placed in T=40-50 DEG C of constant temperature
It is dried overnight in convection oven, then white dried solid particle can be obtained, as cationic dextran based polyalcohol is dry
Powder.
Attached drawing 2 shows the reaction mechanism figure of cationic dextran flocculant in the embodiment of the present invention 1, to dextrose
Potassium peroxydisulfate is added in anhydride solution as radical initiator, is connect in C2 the or C3 carbon potential point with each unit of dextran
Hydroxyl on be also easy to produce hydroxyl radical free radical, and the alkenyl of cationic monomer METAC it is very active and generate more METAC from
By base, becomes the receptor of dextran hydroxyl radical free radical, lead to the chain initiation reaction of dextran-METAC graft copolymer.
Chain initiation is a key link in free radical initiation grafting copolyreaction.Each hydroxyl of dextran unit in the reaction
Base active group can be in graft copolymerization in conjunction with METAC cation.
The Fourier that attached drawing 3 shows cationic dextran flocculant dried powder in the embodiment of the present invention 1 is infrared
Spectrogram.It can see in the spectrogram of dextran, in 3410cm-1The broad peak at place is the O-H base that dextrose units extend
The stretching vibration peak of group, in 2930cm-1Place is C-H stretching vibration peak, and the amorphous areas of dextran, the O-H in conjunction with water are curved
Bent vibration peak is 1650cm-1The absorption peak at place.In 1020cm-1The sharp absorption peak at place is then the α -1 due to dextran,
Caused by 6- glycosidic bond, 860cm-1Place then corresponds to the unique α carbon heterogeneous of dextran compared with strong absworption peak, in 758cm-1The absorption peak at place proves that the configuration should be a typical pyranose ring structure.In modifying process, 3400cm-1The O-H's of left and right
Stretching vibration broad peak intensity is weakened, and illustrates that the associating intensity of hydroxyl weakens.And it is grafted in dextran and the ionization of METAC sun
In the infrared spectroscopy of object, other than the typical structure absorption peak with original dextran, new absorption peak is also added.Its
In, in 1720cm-1The absorption peak at place is the stretching vibration peak of C=O, in 1472cm-1The absorption peak at place is the bending vibration of C-N key
Dynamic peak, in 950cm-1Place is then the characteristic feature absorption peak of quaternary ammonium salt group.The appearance of these new absorption peaks equally also demonstrates
The successful progress of dextran and cationic monomer METAC graft reaction.
The X-ray crystal that attached drawing 4 shows cationic dextran flocculant dried powder in the embodiment of the present invention 1 spreads out
Penetrate figure.Wherein the grafting degree of MDT-1 to MDT-3 product is respectively 75%, 81% and 94%.In dextran map, five
Strong diffraction maximum appear in 2 θ=29 °, 21 ° 19 °, 18 ° 16 ° at there are five sharp strong absworption peak, this is for a α type
X-ray diffraction mode and typical dextran characteristic crystal structure.After graft reaction occurs with cationic monomer METAC,
These characteristic peaks almost disappear, instead the broad peak of more disperse.And with the increase of grafting degree, graft product broad peak
Disperse degree be consequently increased.The generation of this phenomenon destroys the right side mainly due to the introducing of METAC cation graft chain
The intermolecular and intramolecular hydrogen bond in sugared acid anhydride is revolved, causes ordered crystal structure by a degree of destruction.In cation graft
In reaction, radical initiator is that dextran saccharide ring generates big free radical, is occurred with the carbon-carbon double bond of grafted monomers METAC poly-
Reaction is closed, modified-reaction not only occurs on the unformed area of dextran, also gradually changes to the crystal region of dextran.This
Outside, it is easier to be hydrated than orderly crystalline structure due to the amorphous structure of graft, can speculate dextran cation
The solubility for changing derivative is higher than original dextran, can be used as the novel practicability polysaccharide graft flocculant of one kind and is applied to
Water treatment field.
Application examples 1
Graft product obtained above is subjected to the test of kaolin flocculation activity: weighing 2.0g kaolin powder in 1000mL
1~2min is stirred in distilled water, then uses 3~5min of ultrasonic treatment and stands 5min to get concentration is arrived as the height of 2.0g/L
Ridge soil suspension simulated wastewater sample.The cationization dextran graft product fine powder on a small quantity after being strictly dried is weighed,
It is dissolved in the cationic flocculant solution that 0.1% mass fraction is made into a certain amount of distilled water.It is added into Kaolin clay suspension
The cationic flocculant solution of doses, stirs while adding, and stands 5min after continuing 3~5min of stirring.Finally in wavelength
For the absorbance value for measuring supernatant at 550nm, calculates flocculation efficiency F% and is shown below:
F%=(F0-F1)/F0*100%
F0 and F1 is absorbance value of the flocculation front and back kaolin suspension waste water model at OD550 respectively.
It is found by being tested to Kaolin suspension flocculation stirring, pH and dosage are to cationic biological polyoses
The flocculation ability of flocculant has larger impact, and product has extensive pH use scope, and when pH is 6~7, flocculating property is best.It throws
Dosage flocculating property in 0.5~3.15mg/L is preferable, when product dosage is 2mg/L, turbidity is gone to reach 97.8%.Attached drawing
5 be flocculating effect display diagram: aqueous suspension ofkaolin flocculating effect, and a left side is suspension before flocculating, and the right side is after product of the present invention is flocculated
Effect.It is tried it should be noted that the application example uses the kaolin generallyd use when general flocculant performance verification
It tests, but this not just constitutes flocculant of the present invention can only be used to the flocculated limitation of kaolin, because being only this using kaolin
For verifying whether something can be used as the general test that flocculant uses well known to field.Namely flocculant of the invention
Use and be not only limited in the application example 1.
Application examples 2
To sugar refinery sugar-cane juice flocculation application (sugar-cane juice be taken before flocculation from sugar refinery clarification plant liquid): by plus
After the flocculant flocculation for entering doses, the remaining residual solids particle of sugar-cane juice forms biggish settling of floccus in bottom, on
Clear liquid becomes gradually clear.The flocculating conditions such as various dose (10mg/L-90mg/L) are optimized.It was found that working as flocculant
When underdosage, flocculant particle and suspended particulate are not enough to generate enough effective collisions in system, to influence flocculant
Bridge formation effect is formed between molecule and suspended particulate and generates charge neutrality effect carries out flocculating setting.And then when flocculant excess
It will lead to Particle surface charge to increase, the repulsion of like charges increases, the phenomenon steady again of Yi Yinqi system.By calculating sugar-cane juice
Transmissivity after find, the dosage of optimum flocculent is c=70mg/L, and optimal flocculation efficiency can reach 78.1% at this time.Knot
Fruit is as shown in Figure 6.
Claims (10)
1. a kind of preparation method of cationic dextran based polyalcohol, which is characterized in that under anaerobic, to dextrose
Potassium peroxydisulfate is added in anhydride solution and stirs 15-20min, addition METAC reacts 2-4h at 65-75 DEG C, and ethyl alcohol is added and is sunk
It forms sediment, it is dry after purifying washing, obtain white dried solid particle, as cationic dextran based polyalcohol.
2. the preparation method of cationic dextran based polyalcohol as described in claim 1, which is characterized in that the dextrose
Anhydride solution is to obtain sucrose solution by the enzymatic fermentation reaction of dextransucrase.
3. the preparation method of cationic dextran based polyalcohol as claimed in claim 2, which is characterized in that the sucrose is molten
The molar concentration of liquid is 0.55~0.75mol/L, it is obtained using acetic acid-calcium acetate buffer preparation of pH=5.0-5.5
It arrives, the concentration of the dextransucrase is 5.0~6.0U/mL.
4. the preparation method of cationic dextran based polyalcohol as described in claim 1, which is characterized in that the persulfuric acid
The additional amount of potassium is the 3% of dextran quality.
5. the preparation method of cationic dextran based polyalcohol according to claim 1, which is characterized in that described
The molar ratio of METAC and dextran is 3:1.
6. the cationic dextran based polyalcohol that any one of the claim 1-5 preparation method obtains is as flocculant
Using.
7. application as claimed in claim 6, which is characterized in that as application of the flocculant in water pollutant processing.
8. application as claimed in claim 6, which is characterized in that as application of the flocculant in sugar industry.
9. application as claimed in claim 6, which is characterized in that as application of the flocculant in dyestuff contaminant processing.
10. application as claimed in claim 6, which is characterized in that for anions component or had as flocculant
The flocculation treatment of the macromolecular components of anionic group.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112794425A (en) * | 2021-02-05 | 2021-05-14 | 广东省科学院生物工程研究所 | Method for improving flocculation capacity of dextran |
| CN112920404A (en) * | 2021-01-29 | 2021-06-08 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN114014428A (en) * | 2021-12-06 | 2022-02-08 | 山东金洋药业有限公司 | Environment-friendly flocculating agent and application thereof |
| CN114890525A (en) * | 2022-05-19 | 2022-08-12 | 合肥工业大学 | Preparation method and application of dextran-betaine cationic flocculant |
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| JPH06239942A (en) * | 1992-12-17 | 1994-08-30 | Yasuhiko Onishi | Dextran matrix polymer |
| CN104130351A (en) * | 2014-07-23 | 2014-11-05 | 威海汉邦生物环保科技有限公司 | Grafted copolymerized cationic polysaccharide bioflocculant and preparation method thereof |
| CN104861115A (en) * | 2015-02-10 | 2015-08-26 | 中科润蓝环保技术（北京）有限公司 | Preparation method of anionic glucan flocculating agent |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06239942A (en) * | 1992-12-17 | 1994-08-30 | Yasuhiko Onishi | Dextran matrix polymer |
| CN104130351A (en) * | 2014-07-23 | 2014-11-05 | 威海汉邦生物环保科技有限公司 | Grafted copolymerized cationic polysaccharide bioflocculant and preparation method thereof |
| CN104861115A (en) * | 2015-02-10 | 2015-08-26 | 中科润蓝环保技术（北京）有限公司 | Preparation method of anionic glucan flocculating agent |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112920404A (en) * | 2021-01-29 | 2021-06-08 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN112794425A (en) * | 2021-02-05 | 2021-05-14 | 广东省科学院生物工程研究所 | Method for improving flocculation capacity of dextran |
| CN114014428A (en) * | 2021-12-06 | 2022-02-08 | 山东金洋药业有限公司 | Environment-friendly flocculating agent and application thereof |
| CN114890525A (en) * | 2022-05-19 | 2022-08-12 | 合肥工业大学 | Preparation method and application of dextran-betaine cationic flocculant |
| CN114890525B (en) * | 2022-05-19 | 2024-01-23 | 合肥工业大学 | Preparation method and application of dextran-betaine cationic flocculant |
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Application publication date: 20191112 |