CN102134297A - Method for preparing cationic flocculant - Google Patents
Method for preparing cationic flocculant Download PDFInfo
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- CN102134297A CN102134297A CN 201110008204 CN201110008204A CN102134297A CN 102134297 A CN102134297 A CN 102134297A CN 201110008204 CN201110008204 CN 201110008204 CN 201110008204 A CN201110008204 A CN 201110008204A CN 102134297 A CN102134297 A CN 102134297A
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- solute
- cationic flocculant
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- dimethylaminoethyl acrylate
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Abstract
The invention relates to a method for preparing a cationic flocculant and belongs to the technical field of cationic flocculant preparation methods. The method for preparing the cationic flocculant comprises the following steps: 1) adding acrylamide and N,N-dimethylaminoethyl acrylate into water according to a mass ratio of 1:(0.05 to 0.4); 2) under a stirring condition, adding citric acid in an amount which is 30 to 40 percent based on the molar weight of the N,N-dimethylaminoethyl acrylate, adding water and regulating the mass concentration of solute to 15 to 35 percent; 3) adding ethylene diamine tetraacetic acid (EDTA) in an amount which is 50 to 500 ppm of the total mass of the solute, introducing nitrogen at 0 to 40 DEG C, and adding a redox initiator in an amount which is 0.005 to 0.05 times the total mass of the solute and urea in an amount which is 0.1 to 8 percent of the solute in turn; 4) closing a solution system, and initiating a polymerization reaction; and 5) after the reaction is finished, cutting up a sol block, drying and crushing to obtain the product. The method for preparing the cationic flocculant adopts a simple process, is good in use effect and has an obvious effect on removal of heavy metals from sewage.
Description
Technical field
The present invention relates to a kind of cationic flocculant preparation method, belong to flocculation agent preparation method technical field.
Background technology
Organism sewage, as dyeing, papermaking, food-processing and municipal effluent, its mud colloid has negative charge usually, uses cationic flocculant can carry out charge neutralization, and flocculates, thereby reach the purpose that purifies water.
Chinese patent CN1044637 discloses a kind of production method of polymer composite flocculant, it is to be coagulating agent with polymeric aluminum, polymerization iron, and polyvinyl alcohol is the flocculation agent promoting agent, and dredging basic triazine is the precipitation agent of heavy metal, by the artificial addition means of forcing, be combined into polymer composite flocculant again.Complicated component, the manufacturing process complexity.
Chinese patent CN101734772 discloses a kind of composite flocculation agent and preparation method who handles trade effluent, it is a raw material with crystallization iron protochloride, aluminum chloride, sal epsom, zinc chloride, sulfuric acid and potassium permanganate, make through the batch mixing slaking, this composite flocculation agent has most of pollutents such as the suspended substance removed quickly and efficiently in the high-concentration waste water, COD, BOD, colourity, heavy metal, ammonia nitrogen.Same complicated component, the manufacturing process complexity.
Chinese patent CN101560004 discloses hydroximic acid type polymeric flocculant, has the effect of sloughing the heavy metal ion in the sewage.Complicated process of preparation, monomer costs an arm and a leg, and influence is promoted the use of.
Chinese patent CN101327976 discloses a kind of efficient water treatment flocculant that is used for tap water, sewage disposal, comprises the metallic cation flocculation agent, it is characterized in that described high-efficiency sewage flocculant for treating also comprises efficient absorbed component and assistant medicament and composite forming.The composite water treatment agent that forms of this inorganic organic floculant, consumption is greater than pure organic floculant, and the sludge quantity of generation is also big, has increased the sludge disposal cost.Effectively reduce the heavy metal content of sewage, have important Significance for Environment.
Summary of the invention
The objective of the invention is to solve the problem that above-mentioned prior art exists, provide a kind of technology simple, result of use is good, the cationic flocculant preparation method who significantly improves for the heavy metal effect of removing sewage.
A kind of cationic flocculant preparation method of the present invention comprises the steps:
1), add dimethylaminoethyl acrylate in the liquid propene acid amides, wherein the mass ratio of acrylamide and dimethylaminoethyl acrylate is 1: 0.05-0.4;
2), under the agitation condition, add citric acid, the consumption of citric acid is the 0.3-0.4 of dimethylaminoethyl acrylate molar weight, adds water, and adjusting the solute mass concentration is 15-35%;
3) the 50-500ppm EDTA (disodium ethylene diamine tetraacetate) that, adds above-mentioned solute total mass, 0-40 ℃ fed nitrogen 20-40 minute down continuously, purpose is to reach the expeling dissolved oxygen, add solute total mass 0.005-0.05 redox initiator doubly successively, solute total mass 0.1-8% urea;
4), continue to feed nitrogen 10-20 minute, solution system is airtight, the spontaneous intensification of material, initiated polymerization;
5), after reaction finishes, the chopping blob of viscose, oven dry, fragmentation obtains product of the present invention.
Above-mentioned redox initiator is ammonium persulphate, S-WAT, mass ratio 1: 0.5-2.0;
Above-mentioned redox initiator is Potassium Persulphate, sodium formaldehyde sulphoxylate, mass ratio 1: 0.5-2.0.
A kind of cationic flocculant preparation method of the present invention, technology is simple, and result of use is good, and is remarkable for the heavy metal effect of removing sewage.
Embodiment
Below provide the specific embodiment of the present invention, be used for formation of the present invention is further specified.
Embodiment 1
In the 2000mL beaker, add 30% (weight) liquid propene acid amides 500g, add dimethylaminoethyl acrylate 14.3g (0.1mol), add Citric acid monohydrate Food grade 7g (0.033mol), stir, add water, adjusting the solute mass concentration is 20%.The 300ppm EDTA that adds the solute total mass, 10 ℃ fed high pure nitrogen 30 minutes down.
(ammonium persulphate: S-WAT=1: 1), the urea of solute total mass 5% continue to feed nitrogen 15 minutes to add the redox initiator of 0.02 times of solute total mass successively.
Beaker is put in from sealing in the PE plastics bag, and solution system is airtight.The spontaneous intensification of material, initiated polymerization.After reaction in 18 hours finishes, take out the polymer gel piece, the chopping blob of viscose is lower than 80 ℃ of oven dry, and fragmentation obtains product of the present invention.
Embodiment 2
In the 2000mL beaker, add 30% (weight) liquid propene acid amides 600g, add dimethylaminoethyl acrylate 14.3g (0.1mol), add Citric acid monohydrate Food grade 7g (0.033mol), stir, add water, adjusting the solute mass concentration is 35%.The 500ppm EDTA that adds the solute total mass, 15 ℃ fed high pure nitrogen 40 minutes down.
Add successively 0.05 times of solute total mass redox initiator (Potassium Persulphate: sodium formaldehyde sulphoxylate=1: 1), the urea of solute total mass 3.5%.Continue to feed nitrogen 10 minutes.
Beaker is put in from sealing in the PE plastics bag, and solution system is airtight.The spontaneous intensification of material, initiated polymerization.After reaction in 24 hours finishes, take out the polymer gel piece, the chopping blob of viscose is lower than 80 ℃ of oven dry, and fragmentation obtains product of the present invention.
Embodiment 3
In the 2000mL beaker, add 30% (weight) liquid propene acid amides 900g, add dimethylaminoethyl acrylate 14.3g (0.1mol), add Citric acid monohydrate Food grade 6.30g (0.03mol), stir, add water, adjusting the solute mass concentration is 20%.The 400ppm EDTA that adds the solute total mass, 15 ℃ fed high pure nitrogen 20 minutes down.
Add successively 0.005 times of solute total mass redox initiator (Potassium Persulphate: sodium formaldehyde sulphoxylate=1: 2.0), the urea of solute total mass 8.0%.Continue to feed nitrogen 20 minutes.
Beaker is put in from sealing in the PE plastics bag, and solution system is airtight.The spontaneous intensification of material, initiated polymerization.After reaction in 24 hours finishes, take out the polymer gel piece, the chopping blob of viscose is lower than 80 ℃ of oven dry, and fragmentation obtains product of the present invention.
Embodiment 4
In the 2000mL beaker, add 30% (weight) liquid propene acid amides 119g, add dimethylaminoethyl acrylate 14.3g (0.1mol), add Citric acid monohydrate Food grade 8.48g (0.04mol), stir.Add water, adjusting the solute mass concentration is 30%.The 200ppm EDTA that adds the solute total mass, 15 ℃ fed high pure nitrogen 30 minutes down.
Add successively 0.01 times of solute total mass redox initiator (Potassium Persulphate: sodium formaldehyde sulphoxylate=1: 0.5), the urea of solute total mass 0.1%.Continue to feed nitrogen 15 minutes.
Beaker is put in from sealing in the PE plastics bag, and solution system is airtight.The spontaneous intensification of material, initiated polymerization.After reaction in 24 hours finishes, take out the polymer gel piece, the chopping blob of viscose, in 70 ℃ of oven dry, fragmentation obtains product of the present invention.
Embodiment 5
In the 2000mL beaker, add 30% (weight) liquid propene acid amides 300g, add dimethylaminoethyl acrylate 14.3g (0.1mol), add Citric acid monohydrate Food grade 7g (0.033mol), stir, add water, adjust solute mass concentration 15%.The 50ppmEDTA that adds the solute total mass, 0 ℃ fed high pure nitrogen 30 minutes.
Add successively 0.03 times of solute total mass redox initiator (ammonium persulphate: S-WAT=1: 1.2), the urea of solute total mass 0.5%.Continue to feed nitrogen, 15 minutes.
Beaker is put in from sealing in the PE plastics bag, and solution system is airtight.The spontaneous intensification of material, initiated polymerization.After reaction in 24 hours finishes, take out the polymer gel piece, the chopping blob of viscose is lower than 80 ℃ of oven dry, and fragmentation obtains product of the present invention.
Application example
With flocculation agent of the present invention and commercially available cationic flocculant sample, water is dissolved into 2% solution respectively, gets certain municipal effluent and carries out floc test.In the 500ml beaker, add the condensing mud of 200ml, add flocculant solution with the 10ml syringe, each 2ml, the empty beaker of impouring another, and topple over back and forth 8 times.Continue in the mud sample to add the 1ml flocculant solution, repeat aforementioned toppling process, until flocculating effect the best.The add-on of flocculation agent is big and solid with the mud floc sedimentation, and sedimentation is fast, and upper water is limpid to be best.
Mud after the flocculation filters and collects, and drying is weighed.The mud wet method is cleared up, detected contents of heavy metal elements with atomic absorption instrument.
The table 1 flocculation agent experiment effect of disposing of sewage
Flocculation agent of the present invention is handled the sewage of isodose, and the mud dry weight that obtains is suitable with common commercially available flocculation agent, and the heavy metal content of dry state mud is higher, illustrates that the effect of flocculation agent sedimentation removal heavy metal of the present invention improves significantly.
A kind of cationic flocculant preparation method of the above embodiment of the invention, technology is simple, and result of use is good, and is remarkable for the heavy metal effect of removing sewage.
Claims (3)
1. a cationic flocculant preparation method is characterised in that to comprise the steps:
1), add dimethylaminoethyl acrylate in the liquid propene acid amides, the mass ratio of acrylamide and dimethylaminoethyl acrylate is 1: 0.05-0.4;
2), under the agitation condition, add citric acid, the consumption of citric acid is the 0.3-0.4 of dimethylaminoethyl acrylate molar weight, adds water, and adjusting the solute mass concentration is 15-35%;
3), add the 50-500ppm EDTA of solute total mass, 0-40 ℃ feeds nitrogen down and drove away dissolved oxygen in 20-40 minute, adds solute total mass 0.005-0.05 redox initiator doubly successively, the urea of solute total mass 0.1-8%;
4), continue to feed nitrogen 10-20 minute, solution system is airtight, the spontaneous intensification of material, initiated polymerization;
5), after reaction finishes, the chopping blob of viscose, oven dry, fragmentation obtains product of the present invention.
2. according to the described a kind of cationic flocculant preparation method of claim 1, be characterised in that:
Described redox initiator is ammonium persulphate, S-WAT, mass ratio 1: 0.5-2.0.
3. according to the described a kind of cationic flocculant preparation method of claim 1, be characterised in that:
Described redox initiator is Potassium Persulphate, sodium formaldehyde sulphoxylate, mass ratio 1: 0.5-2.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110008204A CN102134297B (en) | 2011-01-07 | 2011-01-07 | Method for preparing cationic flocculant |
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| CN201110008204A CN102134297B (en) | 2011-01-07 | 2011-01-07 | Method for preparing cationic flocculant |
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| CN102134297A true CN102134297A (en) | 2011-07-27 |
| CN102134297B CN102134297B (en) | 2012-10-17 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828922A (en) * | 2015-05-31 | 2015-08-12 | 谢秋鸿 | Preparation method of composite flocculant |
| CN105936581A (en) * | 2016-06-12 | 2016-09-14 | 山东源根化学技术研发有限公司 | Inorganic flocculant, preparation method thereof and inorganic flocculant and papermaking sludge dehydration process using the same |
| CN110182895A (en) * | 2019-05-23 | 2019-08-30 | 中国石油化工股份有限公司 | A kind of degreaser and preparation method thereof for polymer-containing sewage in oil field processing |
| CN111348731A (en) * | 2020-03-10 | 2020-06-30 | 广东海洋大学深圳研究院 | Method for rapidly settling large-particle substances in polluted seawater |
| US10787768B2 (en) | 2016-09-07 | 2020-09-29 | Kemira Oyj | Method for manufacture of paper, board or the like and use of the composition |
| CN112940178A (en) * | 2021-02-03 | 2021-06-11 | 中国海洋石油集团有限公司 | Application of degradable water clarifier |
| CN116135897A (en) * | 2021-11-18 | 2023-05-19 | 郑州大学 | Polyacrylamide copolymer, and preparation method and application thereof |
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| CN1290279A (en) * | 1998-02-06 | 2001-04-04 | Cytec技术有限公司 | Improved polymer blends for dewatering |
| CN101327976A (en) * | 2008-07-15 | 2008-12-24 | 南通立源水处理技术有限公司 | Efficient water treatment flocculant |
| US7473334B2 (en) * | 2004-10-15 | 2009-01-06 | Nalco Company | Method of preparing modified diallyl-N,N-disubstituted ammonium halide polymers |
| CN101456930A (en) * | 2008-12-29 | 2009-06-17 | 郑州正力聚合物科技有限公司 | Cationic polyacrylamide sewage water flocculant |
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2011
- 2011-01-07 CN CN201110008204A patent/CN102134297B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1290279A (en) * | 1998-02-06 | 2001-04-04 | Cytec技术有限公司 | Improved polymer blends for dewatering |
| US7473334B2 (en) * | 2004-10-15 | 2009-01-06 | Nalco Company | Method of preparing modified diallyl-N,N-disubstituted ammonium halide polymers |
| CN101327976A (en) * | 2008-07-15 | 2008-12-24 | 南通立源水处理技术有限公司 | Efficient water treatment flocculant |
| CN101456930A (en) * | 2008-12-29 | 2009-06-17 | 郑州正力聚合物科技有限公司 | Cationic polyacrylamide sewage water flocculant |
Non-Patent Citations (1)
| Title |
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| 《石油化工》 20081231 朱驯等 新型阳离子型絮凝剂聚（N,N-二甲基-N-苄基-N-丙烯酰胺基氯化铵/丙烯酰胺）的合成 90-94 1-3 第37卷, 第1期 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828922A (en) * | 2015-05-31 | 2015-08-12 | 谢秋鸿 | Preparation method of composite flocculant |
| CN105936581A (en) * | 2016-06-12 | 2016-09-14 | 山东源根化学技术研发有限公司 | Inorganic flocculant, preparation method thereof and inorganic flocculant and papermaking sludge dehydration process using the same |
| US10787768B2 (en) | 2016-09-07 | 2020-09-29 | Kemira Oyj | Method for manufacture of paper, board or the like and use of the composition |
| CN110182895A (en) * | 2019-05-23 | 2019-08-30 | 中国石油化工股份有限公司 | A kind of degreaser and preparation method thereof for polymer-containing sewage in oil field processing |
| CN110182895B (en) * | 2019-05-23 | 2021-06-18 | 中国石油化工股份有限公司 | Oil removing agent for polymer-containing sewage treatment in oil field and preparation method thereof |
| CN111348731A (en) * | 2020-03-10 | 2020-06-30 | 广东海洋大学深圳研究院 | Method for rapidly settling large-particle substances in polluted seawater |
| CN112940178A (en) * | 2021-02-03 | 2021-06-11 | 中国海洋石油集团有限公司 | Application of degradable water clarifier |
| CN116135897A (en) * | 2021-11-18 | 2023-05-19 | 郑州大学 | Polyacrylamide copolymer, and preparation method and application thereof |
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| CN102134297B (en) | 2012-10-17 |
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Effective date of registration: 20180523 Address after: 265100 Shandong, Yantai, Penglai City, Daxin store town government residence Patentee after: Penglai star fire Chemical Co., Ltd. Address before: 264006 Kunlun mountain road, Yantai Development Zone, Shandong Province, No. 69 Patentee before: Yantai Development Zone Sparkyt Chemical Co., Ltd. |