CN102617793B - Flocculating agent and preparation method thereof - Google Patents
Flocculating agent and preparation method thereof Download PDFInfo
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- CN102617793B CN102617793B CN201210096508.7A CN201210096508A CN102617793B CN 102617793 B CN102617793 B CN 102617793B CN 201210096508 A CN201210096508 A CN 201210096508A CN 102617793 B CN102617793 B CN 102617793B
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Abstract
The invention provides a preparation method of flocculating agent. The method comprises the steps as follows: acrylamide, acrylic acid, and methyl propene acyl-oxygen ethyl dimethyl benzyl ammonium chloride are dissolved in water so as to obtain mixed solution; the molar ratio of the acrylic acid to the methyl propene acyl-oxygen ethyl dimethyl benzyl ammonium chloride is 1 to (0.5-1.5); and in an inert gas environment, the mixed solution is subjected to polyreaction under the effect of initiating agent, so that the flocculating agent is obtained. In the invention, the contents of positive charge and negative charge in the obtained flocculating agent are the same, the quality of the solution shows an antipolyelectrolyte effect, the performance of the solution cannot change acutely with the increasing of external salt concentration, and the flocculation effect is excellent. Meanwhile, the hydrophobic group carried by the flocculating agent forms physical crosslinking, so that the salt resisting capability of the flocculating agent is enhanced. Therefore, the flocculating effect is improved.
Description
Technical field
The present invention relates to water treatment field, particularly flocculation agent and preparation method thereof.
Background technology
The mixed dispersion of a kind of complicated component that waste water is made up of water and various impurity.Wherein, modal is brine waste.In the production process of multiple industries such as metallurgy, chemical industry, iron and steel, electronics etching, printing and dyeing, food, pharmacy, weaving, chemical industry, Waste water concentrating, product processing, all give off a large amount of high-concentration salt-containing wastewaters, the concentration of some brine waste is up to 10%～25%.In brine waste, except the salt that contains high density, also contain the organism of a large amount of poisonous, difficult degradations, its a large amount of discharges directly cause river water quality salinity to improve, and bring more and more serious pollution to soil, surface water and groundwater.And along with China's rapid development of economy, the quantity discharged of brine waste is the trend of sharp increase, cause great pressure to the ecotope of China.
At present, flocculation agent is widely used at aspects such as wastewater treatment, waste water renewable resources and sludge dewaterings.Flocculation agent can be divided into organic floculant and inorganic flocculating agent according to its chemical composition, and organic floculant comprises again organic polymer coargulator, natural organic high-molecular flocculant and microbial flocculant.In recent years, advantage that sludge quantity that organic polymer coargulator is high with its intrinsic viscosity, adsorption bridging ability is strong, dosage is little, flocculating effect is good, applied widely, produce is few, flocculation rate is fast etc., is widely used in Industrial Wastewater Treatment.
But most organic polymer coargulators are negatively charged ion or cationic polyelectrolyte, intermolecular electrostatic interaction changes polymer chain structure, and then affects flocculating effect.And, adding along with small molecules is electrolytical, the described flocculation of the organic polymer with single electric charge has shielded the electrostatic interaction between like charges, thereby has reduced the hydrodynamic volume of organic polymer coargulator, causes flocculation ability to decline.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of flocculation agent, and flocculation agent provided by the invention has good saline-alkaline tolerance and flocculating effect.
The preparation method who the invention provides a kind of flocculation agent, comprises the following steps:
A) by soluble in water to acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride, obtain mixing solutions;
The mol ratio of described vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride is 1: 0.5～1.5;
B), in inert gas environment, mixing solutions polymerization reaction take place under initiator effect of described step in a), obtains flocculation agent.
Preferably, described step a) in the ratio of vinylformic acid and total amount of substance of methylacryloxyethyldimethyl benzyl ammonium chloride and the amount of substance of acrylamide be 1: 4～20.
Preferably, the initiator of described step in b) is water-soluble azo class initiator or water soluble oxidized reduction series initiators.
Preferably, the initiator of described step in b) is the mixture of azo two isobutyl imidazoline salt hydrochlorates or ammonium persulphate and tetramethyl-diamines.
Preferably, the amount of substance of described initiator and described step a) in the ratio of acrylamide, vinylformic acid and the total amount of substance of methylacryloxyethyldimethyl benzyl ammonium chloride be 0.0005～0.02: 1.
Preferably, described step a) also comprises pH value to 7～9 that regulate described mixing solutions.
Preferably, described step water a) is deionized water.
Preferably, the polymerization time of described step in b) is 12h～24h.
Preferably, the rare gas element of described step in b) is nitrogen or argon gas.
The present invention also provides a kind of flocculation agent of being prepared by method described in technique scheme.
Compared with prior art, the present invention utilizes acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride polymerization reaction take place, obtains flocculation agent.Methylacryloxyethyldimethyl benzyl ammonium chloride has cation group, vinylformic acid has anionic group, the present invention participates in methylacryloxyethyldimethyl benzyl ammonium chloride and vinylformic acid in polymerization with suitable amount of substance, the positive and negative electric charge content of the flocculation agent therefore obtaining is suitable, its SOLUTION PROPERTIES is anti-polyelectrolyte effect, solution property can not increase acute variation, flocculating effect excellence occur with extraneous salt concn.Simultaneously, methylacryloxyethyldimethyl benzyl ammonium chloride also has hydrophobic grouping, during with vinylformic acid and acrylamide polymerization, hydrophobic grouping effect forms physical crosslinking, increase hydrodynamic volume, hydrophobic interaction strengthens with solution polarity, therefore strengthen the saline-alkaline tolerance of flocculation agent, thereby improved its flocculating effect.Experimental result shows, in the polynite of massfraction 1%, adds NaCl, and in the time that NaCl concentration is 0.1mol/L, the flocculation agent that adds 40ppm～100ppm can make turbidity drop to below 10; In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 1mol/L, the flocculation agent that adds 15ppm～60ppm can make turbidity drop to below 10.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The preparation method who the embodiment of the invention discloses a kind of flocculation agent, comprises the following steps:
A) by soluble in water to acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride, obtain mixing solutions;
The mol ratio of described vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride is 1: 0.5～1.5;
B), in inert gas environment, mixing solutions polymerization reaction take place under initiator effect of described step in a), obtains flocculation agent.
The present invention is take acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride as raw material, step a) in by soluble in water to acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride, obtain mixing solutions; The mol ratio of described vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride is 1: 0.5～1.5, is preferably 1: 1.Total amount of substance of described vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride is preferably 1: 4 with the ratio of the amount of substance of acrylamide～and 20, more preferably 1: 8～15.Described water is preferably deionized water.
Obtain after mixing solutions, preferred, also comprise pH value to 7～9 that regulate described mixing solutions.The present invention is not particularly limited the method for the pH value that regulates described mixing solutions, can carry out according to mode well known to those skilled in the art.
Step of the present invention b) in inert gas environment, described mixing solutions is polymerization reaction take place under initiator effect, obtains flocculation agent.
Described initiator is preferably water-soluble azo class initiator or water soluble oxidized reduction series initiators, described water-soluble azo class initiator includes but not limited to azo two isobutyl imidazoline salt hydrochlorates, azo diisobutyl amidine hydrochloride, azo dicyano valeric acid or azo di-isopropyl tetrahydroglyoxaline, is preferably azo two isobutyl imidazoline salt hydrochlorates; While selecting water-soluble azo class initiator, the temperature of described polyreaction is preferably 30 ℃～50 ℃.Described water soluble oxidized reduction series initiators includes but not limited to the mixture of ammonium persulphate and tetramethyl-diamines, and in the mixture of described ammonium persulphate and tetramethyl-diamines, the mol ratio of ammonium persulphate and tetramethyl-diamines is preferably 1～3: 1; While selecting water soluble oxidized reduction series initiators, the temperature of described polyreaction is preferably 5 ℃～20 ℃.The amount of substance of described initiator and described step a) in the ratio of acrylamide, vinylformic acid and the total amount of substance of methylacryloxyethyldimethyl benzyl ammonium chloride be preferably 0.0005～0.02: 1, more preferably 0.001～0.1: 1.Described rare gas element is preferably nitrogen or argon gas.Described polymerization time is preferably 12h～24h, more preferably 15h～20h.
Described mixing solutions after polymerization reaction take place, obtains crude product under initiator effect, and described crude product preferably, through dialysis and acetone precipitation, obtains flocculation agent.
The present invention also provides a kind of flocculation agent of being prepared by method described in technique scheme.
Flocculation agent prepared by the present invention carries out the test of flocculating property, and result shows, in saline solns, and the flocculating effect excellence of flocculation agent; And the increase flocculating property with salt concn strengthens.
The present invention utilizes acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride polymerization reaction take place, obtains flocculation agent.Methylacryloxyethyldimethyl benzyl ammonium chloride has cation group, vinylformic acid has anionic group, the present invention participates in methylacryloxyethyldimethyl benzyl ammonium chloride and vinylformic acid in polymerization with suitable amount of substance, the positive and negative electric charge content of the flocculation agent therefore obtaining is close, its SOLUTION PROPERTIES is anti-polyelectrolyte effect, solution property can not increase acute variation, flocculating effect excellence occur with extraneous salt concn.Simultaneously, methylacryloxyethyldimethyl benzyl ammonium chloride also has hydrophobic grouping, during with vinylformic acid and acrylamide polymerization, hydrophobic grouping effect forms physical crosslinking, increase hydrodynamic volume, hydrophobic interaction strengthens with solution polarity, therefore strengthen the saline-alkaline tolerance of flocculation agent, thereby improved its flocculating effect.
In order further to understand the present invention, below in conjunction with embodiment, flocculation agent provided by the invention and preparation method thereof is described, protection scope of the present invention is not limited by the following examples.
Embodiment 1
To having in the four-hole reaction flask of water of condensation, mechanical stirrer, nitrogen inlet and dropping funnel, 0.18mol acrylamide, 0.01mol vinylformic acid and 0.01mol methylacryloxyethyldimethyl benzyl ammonium chloride are dissolved in 303.62mL deionized water, obtain mixing solutions.The NaOH solution that is 20wt% to mixed solution and dripping mass concentration, adjusts mixing solutions pH value to 8.0.
In mixing solutions, pass into nitrogen 30min, be warming up to 30 ℃, add 0.0002mol azo two isobutyl imidazoline salt hydrochlorates, polyreaction 24h, obtains product.Described product, through dialysis, acetone precipitation, obtains flocculation agent.
The flocculation agent obtaining is carried out to flocculating property test, and result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity is 2000, adds 150ppm flocculation agent and can make suspension turbidity be down to 10 left and right;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 0.1mol/L, the flocculation agent that adds 50ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 1mol/L, the flocculation agent that adds 20ppm can make turbidity drop to 7.
As can be seen here, the flocculation agent obtaining has excellent flocculating effect in salts solution.
Embodiment 2
To having in the four-hole reaction flask of water of condensation, mechanical stirrer, nitrogen inlet and dropping funnel, 0.038mol acrylamide, 0.001mol vinylformic acid and 0.001mol methylacryloxyethyldimethyl benzyl ammonium chloride are dissolved in 97.58mL deionized water, obtain mixing solutions.The NaOH solution that is 20wt% to mixed solution and dripping mass concentration, adjusts mixing solutions pH value to 7.0.
In mixing solutions, pass into nitrogen 30min, be warming up to 50 ℃, add 0.00002mol azo two isobutyl imidazoline salt hydrochlorates, polyreaction 12h, obtains product.Described product, through dialysis, acetone precipitation, obtains flocculation agent.
The flocculation agent obtaining is carried out to flocculating property test, and result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity is 2000, adds 150ppm flocculation agent and can make suspension turbidity be down to 11 left and right;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 0.1mol/L, the flocculation agent that adds 100ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 1mol/L, the flocculation agent that adds 60ppm can make turbidity drop to below 10.
As can be seen here, the flocculation agent obtaining has excellent flocculating effect in salts solution.
Embodiment 3
To having in the four-hole reaction flask of water of condensation, mechanical stirrer, nitrogen inlet and dropping funnel, 0.08mol acrylamide, 0.01mol vinylformic acid and 0.01mol methylacryloxyethyldimethyl benzyl ammonium chloride are dissolved in 102.12mL deionized water, obtain mixing solutions.The NaOH solution that is 20wt% to mixed solution and dripping mass concentration, adjusts mixing solutions pH value to 9.0.
In mixing solutions, pass into nitrogen 30min, be warming up to 15 ℃, add 0.0001mol ammonium persulphate and 0.00005mol Tetramethyl Ethylene Diamine, polyreaction 24h, obtains product.Described product, through dialysis, acetone precipitation, obtains flocculation agent.
The flocculation agent obtaining is carried out to flocculating property test, and result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity is 2000, adds 150ppm flocculation agent and can make suspension turbidity be down to 10 left and right;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 0.1mol/L, the flocculation agent that adds 90ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 1mol/L, the flocculation agent that adds 50ppm can make turbidity drop to 7.
As can be seen here, the flocculation agent obtaining has excellent flocculating effect in salts solution.
Embodiment 4
To having in the four-hole reaction flask of water of condensation, mechanical stirrer, nitrogen inlet and dropping funnel, 0.18mol acrylamide, 0.01mol vinylformic acid and 0.01mol methylacryloxyethyldimethyl benzyl ammonium chloride are dissolved in 303.62mL deionized water, obtain mixing solutions.The NaOH solution that is 20wt% to mixed solution and dripping mass concentration, adjusts mixing solutions pH value to 8.0.
In mixing solutions, pass into nitrogen 30min, put into the ice-water bath of 5 ℃, add 0.0004mol ammonium persulphate and 0.0002mol Tetramethyl Ethylene Diamine, polyreaction 24h, obtains product.Described product, through dialysis, acetone precipitation, obtains flocculation agent.
The flocculation agent obtaining is carried out to flocculating property test, and result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity is 2000, adds 150ppm flocculation agent and can make suspension turbidity be down to 10 left and right;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 0.1mol/L, the flocculation agent that adds 40ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, in the time that NaCl concentration is 1mol/L, the flocculation agent that adds 15ppm can make turbidity drop to 7.
As can be seen here, the flocculation agent obtaining has excellent flocculating effect in salts solution.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple modification of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
1. a preparation method for flocculation agent, comprises the following steps:
A) by soluble in water to acrylamide, vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride, obtain mixing solutions, regulate pH value to 7～9 of described mixing solutions;
The mol ratio of described vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride is 1:0.5～1.5;
B), in inert gas environment, the mixing solutions in described step a) is polymerization reaction take place under initiator effect, obtains flocculation agent.
2. preparation method according to claim 1, is characterized in that, in described step a), the ratio of total amount of substance of vinylformic acid and methylacryloxyethyldimethyl benzyl ammonium chloride and the amount of substance of acrylamide is 1:4～20.
3. preparation method according to claim 1, is characterized in that, the initiator in described step b) is water-soluble azo class initiator or water soluble oxidized reduction series initiators.
4. preparation method according to claim 3, is characterized in that, the initiator in described step b) is the mixture of azo two isobutyl imidazoline salt hydrochlorates or ammonium persulphate and tetramethyl-diamines.
5. preparation method according to claim 3, is characterized in that, in the amount of substance of described initiator and described step a), the ratio of acrylamide, vinylformic acid and the total amount of substance of methylacryloxyethyldimethyl benzyl ammonium chloride is 0.0005～0.02:1.
6. preparation method according to claim 1, is characterized in that, the water of described step a) is deionized water.
7. preparation method according to claim 1, is characterized in that, the polymerization time in described step b) is 12h～24h.
8. preparation method according to claim 1, is characterized in that, the rare gas element in described step b) is nitrogen or argon gas.
9. a flocculation agent of being prepared by the preparation method described in claim 1～8 any one.
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| CN103342778B (en) * | 2013-07-26 | 2015-11-18 | 山东滨州嘉源环保有限责任公司 | A kind of compound salt tolerant hydrophobic association amphoteric flocculating agent and preparation method thereof |
| CN106674422A (en) * | 2016-05-27 | 2017-05-17 | 荆门市拓达科技有限公司 | Painting mist purifying coagulant |
| US11365272B2 (en) * | 2018-05-09 | 2022-06-21 | Jiangnan University | Multi-copolymer, methods for producing the same and using thereof in wastewater treatment |
| CN108559020B (en) * | 2018-05-09 | 2019-05-03 | 江南大学 | A kind of multiple copolymer, preparation method and its application in the treatment of waste water |
| CN111848859B (en) * | 2020-08-14 | 2021-09-14 | 山东大学 | Micro-crosslinked cationic polyacrylamide flocculant and preparation method and application thereof |
| CN115613036A (en) * | 2022-10-11 | 2023-01-17 | 常州大学 | Corrosion inhibitor with flocculation function and preparation method thereof |
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| US5708071A (en) * | 1994-12-15 | 1998-01-13 | Hymo Corporation | Aqueous dispersion of an amphoteric water-soluble polymer, a method of manufacturing the same, and a treating agent comprising the same |
| US5986030A (en) * | 1997-04-15 | 1999-11-16 | Nalco Chemical Company | Fluorescent water soluble polymers |
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