CN105153369A - Amphoteric polysaccharide biological flocculant and preparation method thereof - Google Patents
Amphoteric polysaccharide biological flocculant and preparation method thereof Download PDFInfo
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- CN105153369A CN105153369A CN201510618543.4A CN201510618543A CN105153369A CN 105153369 A CN105153369 A CN 105153369A CN 201510618543 A CN201510618543 A CN 201510618543A CN 105153369 A CN105153369 A CN 105153369A
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- biological flocculant
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- ZIFGYXJHCCWZFM-UHFFFAOYSA-N CCCNC(C)(C)CS(O)(O)O Chemical compound CCCNC(C)(C)CS(O)(O)O ZIFGYXJHCCWZFM-UHFFFAOYSA-N 0.000 description 1
- 0 CC[C@]([C@](*CCN(C)C)O)O* Chemical compound CC[C@]([C@](*CCN(C)C)O)O* 0.000 description 1
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Abstract
The invention provides an amphoteric polysaccharide biological flocculant and a preparation method thereof. A technology of graft copolymerization is adopted, a nonionic type biological flocculant serves as the raw material, cationic monomers, anionic monomers and dissolution additives are added into an aqueous solution of the biological flocculant in sequence at certain water-bath temperature, after a redox initiator is added to be reacted for 1-3 h at the temperature ranging from 35 DEG C to 45 DEG C, the temperature is increased to range from 50 DEG C to 60 DGE C, an azo initiator is added to be reacted for 1-3 h, and the product is finally obtained through sedimentation, water washing, ethanol washing, drying and grinding. According to the amphoteric polysaccharide biological flocculant and the preparation method thereof, the technology of the graft copolymerization is adopted, operation is easy, the reaction conversion rate is high, the cost and effectiveness are stable, the amphoteric polysaccharide biological flocculant and the preparation method thereof are suitable for treating complex and variable water quality and particularly suitable for dehydration of industrial sludge, treatment of landfill leachate, treatment of waste water containing heavy metal, printing and dyeing waste water, oil refining waste water, mineral flotation and the like, and the significant environmental and social benefits are achieved.
Description
Technical field
The invention belongs to polysaccharide bioflocculant modified technique technical field, specifically a kind of amphoteric polysaccharide biological flocculant and preparation method thereof.
Background technology
Along with development that is economic and society, the composition of sewage or waste water is day by day complicated, except containing except electronegative colloidal solid, in water body also containing a lot of metal ion, with the particulate of positive charge or solute, therefore the use of conventional flocculant is restricted greatly, and such as in sludge dewatering, mud itself is with negative charge, due to proceeding of sludge corruption, be used alone cationic flocculant and can cause that the rate of recovery of suspended substance is low, the water ratio of mud cake is high; When the mud processed containing heavy metal or sewage, owing to not only also containing heavy metal substance containing electronegative colloidal solid in water, be just difficult to elimination of colloid stability or metal removal with positively charged ion or anionic flocculant separately, at this time just need amphoteric flocculating agent.
Amphoteric polysaccharide biological flocculant is the one of amphoteric flocculating agent, it on the skeleton of polysaccharide bioflocculant, had both been connected to Cationic functional groups as side base or/and side chain, be connected to again anionic functional group as side base or/and side chain, the quaternary ammonium salt Huo Phosphonium ammonium salt of Cationic functional groups normally containing unsaturated double-bond, anionic functional group normally contains carboxylate salt or the sulfonate of unsaturated double-bond, product has unique electrochemical properties, the synergy of zwitterion functional group can be played, simultaneously by means of the hydroxyl of polysaccharide bioflocculant self, unique molecular chain structure and the molecular weight of superelevation, absorption can better be played, to build bridge and volume such as to sweep at the effect, its synthesis technique is simple, monomer conversion is high, workable, can be used for processing water quality complicated and changeable, be particularly useful for the dehydration of industrial sludge, the process of percolate, the process of heavy metal-containing waste water and dyeing waste water, refinery water, the fields such as mineral floating.
Publication number is the preparation method that the patent of invention of CN102585097A discloses a kind of amphoteric starch, adopting joins in the good starch of gelatinization by cationic monomer, anionic monomer and acrylamide etc., adopt redox initiation system or ceric ammonium nitrate trigger monomer and starch generation graft copolymerization and obtain, wherein cationic monomer comprises dimethyl diallyl ammonium chloride, methyl acyloxyethyl trimethyl ammonium chloride etc., and anionic monomer comprises sodium acrylate, sodium allylsulfonate etc.Publication number is the preparation method that the patent of invention of CN101649006A discloses a kind of amphoteric chitosan, it is by first for chitosan carboxymethylation, through filtering, purify, grafting quaternary ammonium salt monomer again after drying, its carboxymethyl group adopts cyclic acid anhydride as MALEIC ANHYDRIDE, Pyroglutaric acid etc., quaternary ammonium salt then selects 2, 3-epoxypropyltrimethylchloride chloride and 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, although cyclic acid anhydride used decreases corrodibility and the spacerarm extending main chain and carboxyl is conducive to the carrying out of reaction kinetic, but there is many washings in the reaction that this distribution is carried out, purify, the complex process techniques such as drying, and selected alcohols material as solvent.Publication number is the preparation method that CN103497279A discloses a kind of amphoteric fibers cellulosic material, it is first quaternised modified by carrying out after Mierocrystalline cellulose alkalinisation treatment, mainly chloro-for 3-2 hydroxypropyl-trimethyl ammonium chlorides are combined with Mierocrystalline cellulose as etherifying agent, cause the graft copolymerization with cellulose skeleton with 2-acrylamide-2-methyl propane sulfonic by ceric ammonium nitrate afterwards.
Except the amphoterisation process to natural polysaccharide macromolecular materials such as starch, chitosan and Mierocrystalline celluloses, also has the modification to guar gum, trimethyl-glycine, bagasse xylan etc., these modifications are mostly by the impact of the performance of polysaccharide material own, need to do polystep reaction and strict process for separating and purifying, and need a lot of organic solvent to add the intractability of waste liquid, and molecular weight is not high.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of amphoteric polysaccharide biological flocculant and preparation method thereof, it is nontoxic, the environmental protection with ultra-high molecular weight that adopts the enzyme method technique of original creation to obtain and biodegradable non-ionic type polysaccharide polymer is raw material, by graft copolymerization technique, make its monomer being simultaneously connected to positively charged ion and negatively charged ion or self-aggregate as side chain or side base, give the flocculating property of its uniqueness.
The technical solution adopted for the present invention to solve the technical problems is:
The invention provides a kind of amphoteric polysaccharide biological flocculant, its skeleton symbol is:
Wherein:
The present invention also provides a kind of preparation method of amphoteric polysaccharide biological flocculant, with non-ionic type polysaccharide bioflocculant solution for raw material, adopt the technique of graft copolymerization obtain both with Cationic functional groups also with the amphoteric polysaccharide biological flocculant of anionic functional group, concrete steps are: in non-ionic type biofloculation agent solution, add cation mono liquid solution respectively, anionic monomer solution and dissolution aids, redox initiator reaction 1-3h is added at 35-45 DEG C, then 50-60 DEG C is warming up to, add azo-initiator reaction 1-3h, reaction product is through alcohol wash, washing, alcohol wash, dry, the final obtained described amphoteric polysaccharide biological flocculant of grinding.
Preferably, the skeleton symbol of described non-ionic type polysaccharide bioflocculant is:
Wherein n=1000 ~ 200000.
The preparation method of described non-ionic type polysaccharide bioflocculant is preferably Patent publication No for a kind of Enzymology method preparing polysaccharide bioflocculant described in CN101392280A, and its concrete preparation method is as follows:
The preferred kinetic viscosity of described polysaccharide bioflocculant is respectively 4500cPs and 11250cPs, comprises following making step:
(1) according to the requirement of above-mentioned polysaccharide bioflocculant kinetic viscosity, compound concentration is the sucrose solution 1000 milliliters of 0.80mol/L and 0.73mol/L and 5000 milliliters accordingly respectively;
(2) in above-mentioned sucrose solution, add calcium chloride solution respectively, wherein concentration be add respectively in the solution of 0.80mol/L and 0.73mol/L 0.5% calcium chloride solution 10 milliliters and 50 milliliters;
(3) regulate the pH value of above-mentioned sucrose solution in 5.2 ~ 5.4 scopes with 30% hac buffer;
(4) in above-mentioned sucrose solution, add dextransucrase solution 17.5 milliliters and 109.6 milliliters respectively, the activity of enzyme is respectively 456IU/ml and 456IU/ml, after mixing, by 10% acetic acid adjust ph in 5.2 ~ 5.4 scopes;
(5) above-mentioned solution is placed in water bath with thermostatic control, regulate and stir, abundant reaction is until solution reaches required kinetic viscosity, and the water bath with thermostatic control temperature that the solution of above-mentioned 0.80mol/L and 0.73mol/L two kinds of different concns is corresponding is respectively 20 ~ 22 DEG C and 22 ~ 24 DEG C;
(6) heat sterilization is carried out to reaction product, filtering and impurity removing, after purified concentration, namely obtain described non-ionic type polysaccharide bioflocculant.
Preferably, described non-ionic type biological flocculant is 1:1-1:6 with the solid masses ratio of all monomers, cationic monomer compares 1:4-4:1 with the solid masses of anionic monomer, the mass percentage that dissolution aids accounts for reaction system is 10-30%, the interpolation quality of redox initiator and azo-initiator all accounts for the 1-5 ‰ of total reactant quality, and wherein the mass ratio of Oxidizing and Reducing Agents is 1:1-2:1.
Preferably, described cationic monomer is any one in acrylyl oxy-ethyl-trimethyl salmiac (DAC), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC), dimethylaminoethyl acrylate (DMAEA), dimethylaminoethyl methacrylate (DMAEMA), acryloxyethyldimethyl benzyl ammonium chloride (DBC), methylacryloxyethyldimethyl benzyl ammonium chloride (DMBC);
Preferably, described anionic monomer is any one sodium salt in vinylformic acid, methacrylic acid, toxilic acid, fumaric acid, 2-acrylamide-2-methylpro panesulfonic acid, methyl propane sulfonic acid, propanesulfonic acid or sylvite;
Preferably, described dissolution aids is any one in urea, ammonium sulfate, sodium sulfate, sodium-chlor, ammonium chloride;
Preferably, in described redox initiator, oxygenant is any one in Potassium Persulphate, Sodium Persulfate and ammonium persulphate, and reductive agent is any one in sodium bisulfite, S-WAT, Potassium hydrogen sulfite, potassium sulfite, ammonium bisulfite, ammonium sulphite;
Preferably, described azo-initiator is: azo diisobutyl amidine (AIBA) or azo di-isopropyl imidazoline hydrochloride (AIBI).
Described its reaction principle of amphoteric polysaccharide biological flocculant is as follows:
Wherein:
Remarkable advantage of the present invention is:
First, product appearance of the present invention is pale yellow powder, product is nontoxic, environmental protection, efficient, belong to the modified product of polysaccharide bioflocculant, different from the modification of the both sexes products such as current starch based, cellulose family, chitosan class, the substep of employing adds different initiators, can ensure that cationic monomer and anionic monomer with polysaccharide bioflocculant skeleton, sufficient graft reaction can occur, simple to operate, monomer conversion is high, and stable performance.
Secondly, product of the present invention has unique chemical property, be particularly useful for water quality complexity, the clean water treatment of the colloid simultaneously containing different electric charge, solvend and heavy metal, owing to not containing monomer or the polymkeric substance of the poly-inorganic salt such as aluminium, Polyferric Sulfate and acrylamide, so there are not the problems such as residual of the large and toxic monomers of metal residual, corrosion pipeline, sludge output in water, can be used for the fields such as the dehydration of industrial sludge, the process of percolate, the process of heavy metal-containing waste water and dyeing waste water, refinery water, mineral floating.Its flocculating effect is excellent, nontoxic, environmental protection, biodegradable, has market outlook and good economic results in society widely.
Embodiment
Below to a preferred embodiment of the present invention will be described in detail.
Embodiment 1
Preparation 2-acrylamide-2-methylpro panesulfonic acid sodium water solution: by massfraction be 50% the 2-acrylamide-2-methylpro panesulfonic acid aqueous solution be placed in ice-water bath, toward wherein slowly drip mass concentration be the aqueous sodium hydroxide solution of 30%, the pH of final solution is 7-8.
The non-ionic type polysaccharide bioflocculant that 200g mass concentration is 15% is added in 500ml there-necked flask, then MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) the solution 75g that mass concentration is 80% is added successively, mass concentration is the 2-acrylamide-2-methylpro panesulfonic acid sodium water solution 142.86g of 42%, urea 15g, start stirring, then pass into nitrogen and be about 20min, be warming up to 40 DEG C, add Potassium Persulphate 0.3g, sodium bisulfite 0.3g, after reaction 1h, be warming up to 50 DEG C, add azo diisobutyl amidine 0.15g, reaction 2h, take out afterwards, through alcohol wash, washing, after alcohol wash and drying and grinding, obtained amphoteric polysaccharide biological flocculant.
Embodiment 2
Preparation degree of neutralization is the Acrylic Acid Monomer solution of 80%: take 100g vinylformic acid and 44.4g sodium hydroxide, vinylformic acid is placed in ice-water bath, sodium hydroxide is dissolved in the water of 150ml, after cooling, slowly instill in vinylformic acid, drip while stir, can reach the Acrylic Acid Monomer solution that degree of neutralization is 80%, monomer whose content is 34.2%.
The polysaccharide bioflocculant that 100g concentration is 15% is added in 500ml there-necked flask, then methylacryloxyethyldimethyl benzyl ammonium chloride (DMBC) the solution 50g that concentration is 60% is added successively, concentration is the vinylformic acid of 34.2% and the mixed aqueous solution 87.72g of sodium acrylate, urea 15g, start stirring, then pass into nitrogen and be about 20min, be warming up to 40 DEG C, add ammonium persulphate 0.15g, S-WAT 0.15g, after reaction 2h, be warming up to 60 DEG C, add azo diisobutyl amidine 0.15g, reaction 1h, take out afterwards, through alcohol wash, washing, after alcohol wash and drying and grinding, obtained amphoteric polysaccharide biological flocculant.
Embodiment 3
Toward in 500ml there-necked flask, add the polysaccharide bioflocculant that 100g concentration is 14.4%, then acrylyl oxy-ethyl-trimethyl salmiac (DAC) the solution 72g that concentration is 60% is added, then methyl propane sulfonic acid sodium 21.6g is added, then add 23.76g dissolution aids ammonium chloride and start stirring, then pass into nitrogen and be about 20min, be warming up to 40 DEG C, add ammonium persulphate 0.198g, sodium bisulfite 0.198g, after reaction 2h, be warming up to 60 DEG C, add azo diisobutyl amidine 0.16g, reaction 2h, take out afterwards, through alcohol wash, washing, after alcohol wash and drying and grinding, obtained amphoteric polysaccharide biological flocculant.
Above-describedly be only the preferred embodiments of the present invention; be understood that; the explanation of above embodiment just understands method of the present invention and core concept thereof for helping; the protection domain be not intended to limit the present invention; all any amendments, equivalent replacement etc. made within thought of the present invention and principle, all should be included within protection scope of the present invention.
Claims (9)
1. an amphoteric polysaccharide biological flocculant, is characterized in that: its skeleton symbol is:
Wherein:
。
2. the preparation method of amphoteric polysaccharide biological flocculant described in a claim 1, it is characterized in that: with non-ionic type polysaccharide bioflocculant solution for raw material, adopt the technique of graft copolymerization obtain both with Cationic functional groups also with the amphoteric polysaccharide biological flocculant of anionic functional group, concrete steps are: in non-ionic type biofloculation agent solution, add cation mono liquid solution respectively, anionic monomer solution and dissolution aids, redox initiator reaction 1-3h is added at 35-45 DEG C, then 50-60 DEG C is warming up to, add azo-initiator reaction 1-3h, reaction product is through alcohol wash, washing, alcohol wash, dry, the final obtained described amphoteric polysaccharide biological flocculant of grinding.
3. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, is characterized in that: the skeleton symbol of described non-ionic type polysaccharide bioflocculant is:
Wherein n=1000 ~ 200000.
4. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, it is characterized in that: described non-ionic type biological flocculant is 1:1-1:6 with the solid masses ratio of all monomers, cationic monomer compares 1:4-4:1 with the solid masses of anionic monomer, the mass percentage that dissolution aids accounts for reaction system is 10-30%, the interpolation quality of redox initiator and azo-initiator all accounts for the 1-5 ‰ of total reactant quality, and wherein the mass ratio of Oxidizing and Reducing Agents is 1:1-2:1.
5. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, is characterized in that: described cationic monomer is any one in acrylyl oxy-ethyl-trimethyl salmiac (DAC), MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC), dimethylaminoethyl acrylate (DMAEA), dimethylaminoethyl methacrylate (DMAEMA), acryloxyethyldimethyl benzyl ammonium chloride (DBC), methylacryloxyethyldimethyl benzyl ammonium chloride (DMBC).
6. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, is characterized in that: described anionic monomer is any one sodium salt in vinylformic acid, methacrylic acid, toxilic acid, fumaric acid, 2-acrylamide-2-methylpro panesulfonic acid, methyl propane sulfonic acid, propanesulfonic acid or sylvite.
7. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, is characterized in that: described dissolution aids is any one in urea, ammonium sulfate, sodium sulfate, sodium-chlor, ammonium chloride.
8. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, it is characterized in that: in described redox initiator, oxygenant is any one in Potassium Persulphate, Sodium Persulfate and ammonium persulphate, reductive agent is any one in sodium bisulfite, S-WAT, Potassium hydrogen sulfite, potassium sulfite, ammonium bisulfite, ammonium sulphite.
9. the preparation method of a kind of amphoteric polysaccharide biological flocculant according to claim 2, is characterized in that: described azo-initiator is: azo diisobutyl amidine (AIBA) or azo di-isopropyl imidazoline hydrochloride (AIBI).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110950521A (en) * | 2019-11-08 | 2020-04-03 | 威海汉邦生物环保科技股份有限公司 | Chemical treatment method for improving red mud settling separation effect |
| CN112920404A (en) * | 2021-01-29 | 2021-06-08 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN115108619A (en) * | 2021-03-23 | 2022-09-27 | 东莞理工学院 | Slurry sewage flocculant and preparation method thereof |
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| CN102250291A (en) * | 2011-05-25 | 2011-11-23 | 何善媛 | Ampholytic modified grafted starch flocculant |
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2015
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| CN101392280A (en) * | 2007-09-18 | 2009-03-25 | 庄茅 | Enzymology method for preparing polysaccharide bioflocculant |
| CN102250291A (en) * | 2011-05-25 | 2011-11-23 | 何善媛 | Ampholytic modified grafted starch flocculant |
| CN103889395A (en) * | 2011-11-04 | 2014-06-25 | 阿克佐诺贝尔化学国际公司 | Graft dendrite copolymers, and methods for producing the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110950521A (en) * | 2019-11-08 | 2020-04-03 | 威海汉邦生物环保科技股份有限公司 | Chemical treatment method for improving red mud settling separation effect |
| CN110950521B (en) * | 2019-11-08 | 2021-11-09 | 威海汉邦生物环保科技股份有限公司 | Chemical treatment method for improving red mud settling separation effect |
| CN112920404A (en) * | 2021-01-29 | 2021-06-08 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN112920404B (en) * | 2021-01-29 | 2023-01-24 | 合肥工业大学 | Preparation method and application of dextran-polyamino acid cationic flocculant |
| CN115108619A (en) * | 2021-03-23 | 2022-09-27 | 东莞理工学院 | Slurry sewage flocculant and preparation method thereof |
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Application publication date: 20151216 |