CN102617793A - Flocculating agent and preparation method thereof - Google Patents
Flocculating agent and preparation method thereof Download PDFInfo
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- CN102617793A CN102617793A CN2012100965087A CN201210096508A CN102617793A CN 102617793 A CN102617793 A CN 102617793A CN 2012100965087 A CN2012100965087 A CN 2012100965087A CN 201210096508 A CN201210096508 A CN 201210096508A CN 102617793 A CN102617793 A CN 102617793A
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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.Concentrate at metallurgy, chemical industry, iron and steel, electronics etching, printing and dyeing, food, pharmacy, weaving, chemical industry, waste water, all give off the great deal of high concentration brine waste in the production process of a plurality of industries such as product processing, the concentration of some brine waste is up to 10%～25%.Except that the salt that contains high density, also contain the organism of a large amount of poisonous, difficult degradations in the brine waste, its a large amount of dischargings directly cause the river water quality salinity to improve, and bring more and more serious pollution for soil, surface water and underground water.And along with China's rapid development of economy, the quantity discharged of brine waste is the trend of sharp increase, has caused great pressure for 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 ingredients, and organic floculant comprises organic polymer coargulator, natural organic high-molecular flocculant and microbial flocculant again.In recent years, organic polymer coargulator is widely used in Industrial Wastewater Treatment with advantages such as the sludge quantity that its intrinsic viscosity is high, the adsorption bridging ability is strong, dosage is little, flocculating effect is good, applied widely, produce are few, flocculation rate is fast.
Yet most organic polymer coargulators are negatively charged ion or cationic polyelectrolyte, and intermolecular electrostatic interaction changes the polymer chain structure, and then influences flocculating effect.And along with the electrolytical adding of small molecules, the said organic polymer flocculation that has 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 descend.
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 invention provides a kind of preparation method of flocculation agent, may further comprise the steps:
A) acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is soluble in water, obtain mixing solutions;
The mol ratio of said vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 1: 0.5～1.5;
B) in inert gas environment, the mixing solutions in the said step a) is polymerization reaction take place under the initiator effect, obtains flocculation agent.
Preferably, the ratio of total amount of substance of vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride and the amount of substance of acrylic amide is 1: 4～20 in the said step a).
Preferably, the initiator in the said step b) is water-soluble azo class initiator or water soluble oxidized reduction series initiators.
Preferably, the initiator in the said step b) is the mixture of azo two isobutyl imidazoline salt hydrochlorates or ammonium persulphate and tetramethyl-diamines.
Preferably, the ratio of acrylic amide, vinylformic acid and the total amount of substance of methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 0.0005～0.02: 1 in the amount of substance of said initiator and the said step a).
Preferably, said step a) also comprises pH value to 7～9 of regulating said mixing solutions.
Preferably, the water of said step a) is deionized water.
Preferably, the polymerization time in the said step b) is 12h～24h.
Preferably, the rare gas element in the said step b) is nitrogen or argon gas.
The present invention also provides a kind of flocculation agent by the said method preparation of technique scheme.
Compared with prior art, the present invention utilizes acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride polymerization reaction take place, obtains flocculation agent.The methylacryoyloxyethyl dimethyl benzyl ammonium chloride has cation group; Vinylformic acid has anionic group; The present invention participates in methylacryoyloxyethyl dimethyl benzyl ammonium chloride and vinylformic acid in polymerization with suitable amount of substance, and the positive and negative electric charge content of the flocculation agent that therefore obtains is suitable, and its SOLUTION PROPERTIES is anti-polyelectrolyte effect; Acute variation can not take place with extraneous salt concn increase in solution property, and flocculating effect is excellent.Simultaneously; The methylacryoyloxyethyl dimethyl benzyl ammonium chloride also has hydrophobic grouping; The hydrophobic grouping effect forms physical crosslinking during with vinylformic acid and acrylamide polymerization, has increased hydrodynamic volume, and 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 when NaCl concentration was 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, when NaCl concentration was 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, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of preparation method of flocculation agent, may further comprise the steps:
A) acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is soluble in water, obtain mixing solutions;
The mol ratio of said vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 1: 0.5～1.5;
B) in inert gas environment, the mixing solutions in the said step a) is polymerization reaction take place under the initiator effect, obtains flocculation agent.
The present invention is a raw material with acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride, and is in the step a) that acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is soluble in water, obtains mixing solutions; The mol ratio of said vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 1: 0.5～1.5, is preferably 1: 1.Total amount of substance of said vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is preferably 1: 4 with the ratio of the amount of substance of acrylic amide～and 20, more preferably 1: 8～15.Said water is preferably deionized water.
After obtaining mixing solutions, preferred, also comprise pH value to 7～9 of regulating said mixing solutions.The present invention does not have particular restriction to the method for the pH value of regulating said mixing solutions, can carry out according to mode well known to those skilled in the art.
In inert gas environment, said mixing solutions is polymerization reaction take place under the initiator effect, obtains flocculation agent in step b) of the present invention.
Said initiator is preferably water-soluble azo class initiator or water soluble oxidized reduction series initiators; Said 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; When selecting water-soluble azo class initiator for use, the temperature of said polyreaction is preferably 30 ℃～50 ℃.Said water soluble oxidized reduction series initiators includes but not limited to the mixture of ammonium persulphate and tetramethyl-diamines, and in the mixture of said ammonium persulphate and tetramethyl-diamines, the mol ratio of ammonium persulphate and tetramethyl-diamines is preferably 1～3: 1; When selecting water soluble oxidized reduction series initiators for use, the temperature of said polyreaction is preferably 5 ℃～20 ℃.The ratio of acrylic amide, vinylformic acid and the total amount of substance of methylacryoyloxyethyl dimethyl benzyl ammonium chloride is preferably 0.0005～0.02: 1 in the amount of substance of said initiator and the said step a), and more preferably 0.001～0.1: 1.Said rare gas element is preferably nitrogen or argon gas.Said polymerization time is preferably 12h～24h, more preferably 15h～20h.
Said mixing solutions obtains crude product behind polymerization reaction take place under the initiator effect, said crude product preferably through dialysis and acetone precipitation, obtains flocculation agent.
The present invention also provides a kind of flocculation agent by the said method preparation of technique scheme.
Flocculation agent to the present invention's preparation carries out the test of flocculating property, and the result shows that in saline solns, the flocculating effect of flocculation agent is excellent; And the increase flocculating property with salt concn strengthens.
The present invention utilizes acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride polymerization reaction take place, obtains flocculation agent.The methylacryoyloxyethyl dimethyl benzyl ammonium chloride has cation group; Vinylformic acid has anionic group; The present invention participates in methylacryoyloxyethyl dimethyl benzyl ammonium chloride and vinylformic acid in polymerization with suitable amount of substance, and the positive and negative electric charge content of the flocculation agent that therefore obtains is close, and its SOLUTION PROPERTIES is anti-polyelectrolyte effect; Acute variation can not take place with extraneous salt concn increase in solution property, and flocculating effect is excellent.Simultaneously; The methylacryoyloxyethyl dimethyl benzyl ammonium chloride also has hydrophobic grouping; The hydrophobic grouping effect forms physical crosslinking during with vinylformic acid and acrylamide polymerization, has increased hydrodynamic volume, and 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
In four-hole reaction flask with water of condensation, mechanical stirrer, nitrogen inlet and tap funnel; 0.18mol acrylic amide, 0.01mol vinylformic acid and 0.01mol methylacryoyloxyethyl dimethyl benzyl ammonium chloride are dissolved in the 303.62mL deionized water, obtain mixing solutions.To the mixed solution and dripping mass concentration is the NaOH solution of 20wt%, adjustment mixing solutions pH value to 8.0.
In mixing solutions, feed nitrogen 30min, be warming up to 30 ℃, add 0.0002mol azo two isobutyl imidazoline salt hydrochlorates, polyreaction 24h obtains product.Said product obtains flocculation agent through dialysis, acetone precipitation.
The flocculation agent that obtains is carried out the flocculating property test, and the result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity are 2000, add the 150ppm flocculation agent suspension-s turbidity is reduced to about 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 0.1mol/L, the flocculation agent that adds 50ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 1mol/L, the flocculation agent that adds 20ppm can make turbidity drop to 7.
This shows that the flocculation agent that obtains has excellent flocculating effect in salts solution.
Embodiment 2
In four-hole reaction flask with water of condensation, mechanical stirrer, nitrogen inlet and tap funnel; 0.038mol acrylic amide, 0.001mol vinylformic acid and 0.001mol methylacryoyloxyethyl dimethyl benzyl ammonium chloride are dissolved in the 97.58mL deionized water, obtain mixing solutions.To the mixed solution and dripping mass concentration is the NaOH solution of 20wt%, adjustment mixing solutions pH value to 7.0.
In mixing solutions, feed nitrogen 30min, be warming up to 50 ℃, add 0.00002mol azo two isobutyl imidazoline salt hydrochlorates, polyreaction 12h obtains product.Said product obtains flocculation agent through dialysis, acetone precipitation.
The flocculation agent that obtains is carried out the flocculating property test, and the result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity are 2000, add the 150ppm flocculation agent suspension-s turbidity is reduced to about 11;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 0.1mol/L, the flocculation agent that adds 100ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 1mol/L, the flocculation agent that adds 60ppm can make turbidity drop to below 10.
This shows that the flocculation agent that obtains has excellent flocculating effect in salts solution.
Embodiment 3
In four-hole reaction flask with water of condensation, mechanical stirrer, nitrogen inlet and tap funnel; 0.08mol acrylic amide, 0.01mol vinylformic acid and 0.01mol methylacryoyloxyethyl dimethyl benzyl ammonium chloride are dissolved in the 102.12mL deionized water, obtain mixing solutions.To the mixed solution and dripping mass concentration is the NaOH solution of 20wt%, adjustment mixing solutions pH value to 9.0.
In mixing solutions, feed nitrogen 30min, be warming up to 15 ℃, add 0.0001mol ammonium persulphate and 0.00005mol Tetramethyl Ethylene Diamine, polyreaction 24h obtains product.Said product obtains flocculation agent through dialysis, acetone precipitation.
The flocculation agent that obtains is carried out the flocculating property test, and the result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity are 2000, add the 150ppm flocculation agent suspension-s turbidity is reduced to about 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 0.1mol/L, the flocculation agent that adds 90ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 1mol/L, the flocculation agent that adds 50ppm can make turbidity drop to 7.
This shows that the flocculation agent that obtains has excellent flocculating effect in salts solution.
Embodiment 4
In four-hole reaction flask with water of condensation, mechanical stirrer, nitrogen inlet and tap funnel; 0.18mol acrylic amide, 0.01mol vinylformic acid and 0.01mol methylacryoyloxyethyl dimethyl benzyl ammonium chloride are dissolved in the 303.62mL deionized water, obtain mixing solutions.To the mixed solution and dripping mass concentration is the NaOH solution of 20wt%, adjustment mixing solutions pH value to 8.0.
In mixing solutions, feed nitrogen 30min, put into 5 ℃ ice-water bath, add 0.0004mol ammonium persulphate and 0.0002mol Tetramethyl Ethylene Diamine, polyreaction 24h obtains product.Said product obtains flocculation agent through dialysis, acetone precipitation.
The flocculation agent that obtains is carried out the flocculating property test, and the result shows:
The montmorillonite suspension liquid of massfraction 1%, turbidity are 2000, add the 150ppm flocculation agent suspension-s turbidity is reduced to about 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 0.1mol/L, the flocculation agent that adds 40ppm can make turbidity drop to below 10;
In the polynite of massfraction 1%, add NaCl, when NaCl concentration was 1mol/L, the flocculation agent that adds 15ppm can make turbidity drop to 7.
This shows that the flocculation agent that obtains has excellent flocculating effect in salts solution.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle 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 claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. the preparation method of a flocculation agent may further comprise the steps:
A) acrylic amide, vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is soluble in water, obtain mixing solutions;
The mol ratio of said vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 1: 0.5～1.5;
B) in inert gas environment, the mixing solutions in the said step a) is polymerization reaction take place under the initiator effect, obtains flocculation agent.
2. preparation method according to claim 1 is characterized in that, total amount of substance of vinylformic acid and methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 1: 4～20 with the ratio of the amount of substance of acrylic amide in the said step a).
3. preparation method according to claim 1 is characterized in that, the initiator in the said 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 the said 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, the ratio of acrylic amide, vinylformic acid and the total amount of substance of methylacryoyloxyethyl dimethyl benzyl ammonium chloride is 0.0005～0.02: 1 in the amount of substance of said initiator and the said step a).
6. preparation method according to claim 1 is characterized in that, said step a) also comprises pH value to 7～9 of regulating said mixing solutions.
7. preparation method according to claim 1 is characterized in that, the water of said step a) is deionized water.
8. preparation method according to claim 1 is characterized in that, the polymerization time in the said step b) is 12h～24h.
9. preparation method according to claim 1 is characterized in that, the rare gas element in the said step b) is nitrogen or argon gas.
10. flocculation agent by any described preparation method preparation of claim 1～9.
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| CN103342778A (en) * | 2013-07-26 | 2013-10-09 | 山东滨州嘉源环保有限责任公司 | Composite salt-tolerant hydrophobic associated amphoteric flocculant 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 |
| CN108559020A (en) * | 2018-05-09 | 2018-09-21 | 江南大学 | A kind of multiple copolymer, preparation method and its application in the treatment of waste water |
| WO2019213868A1 (en) * | 2018-05-09 | 2019-11-14 | 江南大学 | Multi-copolymer, preparation method therefor and application thereof in wastewater treatment |
| CN111848859A (en) * | 2020-08-14 | 2020-10-30 | 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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| CN111848859A (en) * | 2020-08-14 | 2020-10-30 | 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 |
| CN115613036B (en) * | 2022-10-11 | 2024-05-03 | 常州大学 | Corrosion inhibitor with flocculation effect and preparation method thereof |
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